#------------------------------------------------------------------------------
#$Date: 2025-07-06 18:43:28 +0200 (Sun 06 de Jul de 2025) $
#$Revision: 300922 $
#$URL: svn://www.crystallography.net/cod/cif/7/71/83/7718308.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_7718308
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            'Ce3 I S6.61 Se1.39 Si2'
_chemical_formula_weight         925.11
_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                 97.5980(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.0737(3)
_cell_length_b                   7.89400(10)
_cell_length_c                   10.9299(2)
_cell_measurement_reflns_used    9321
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      32.53
_cell_measurement_theta_min      2.56
_cell_volume                     1374.67(4)
_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      298(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.999
_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  0.0280
_diffrn_reflns_av_unetI/netI     0.0095
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            38987
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.503
_diffrn_reflns_theta_min         2.557
_diffrn_source                   'fine-focus seald tube'
_exptl_absorpt_coefficient_mu    16.827
_exptl_absorpt_correction_T_max  0.4950
_exptl_absorpt_correction_T_min  0.3601
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'multi-scan (SADABS" Sheldrick, 2016/2)'
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    4.470
_exptl_crystal_description       Rod
_exptl_crystal_F_000             1632
_exptl_crystal_size_max          0.072
_exptl_crystal_size_mid          0.036
_exptl_crystal_size_min          0.031
_refine_diff_density_max         1.088
_refine_diff_density_min         -0.582
_refine_diff_density_rms         0.094
_refine_ls_extinction_coef       0.000111(18)
_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   1.078
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     70
_refine_ls_number_reflns         2099
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.078
_refine_ls_R_factor_all          0.0106
_refine_ls_R_factor_gt           0.0095
_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)+(0.0063P)²+3.7284P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0216
_refine_ls_wR_factor_ref         0.0221
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2010
_reflns_number_total             2099
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d4dt03506b2.cif
_cod_data_source_block           GP1077A2_OSW2
_cod_depositor_comments
'Adding full bibliography for 7718307--7718310.cif.'
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               7718308
_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   0.377
_shelx_estimated_absorpt_t_max   0.624
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
Ce1 Ce 0.30182(2) 0.12028(2) 0.31787(2) 0.01212(3) Uani 1 1 d . . . . .
Ce2 Ce 0.000000 0.09532(2) 0.250000 0.01413(4) Uani 1 2 d S T P . .
I1 I 0.000000 0.51382(2) 0.250000 0.02621(5) Uani 1 2 d S T P A .
S1 S 0.06558(2) 0.15962(4) 0.54266(3) 0.01447(9) Uani 0.6012(18) 1 d . . P A 8
S3 S 0.21723(2) 0.43140(5) 0.41537(3) 0.01295(11) Uani 0.8785(17) 1 d . . P B 10
S2 S 0.14422(2) 0.24640(5) 0.14602(3) 0.01402(11) Uani 0.8734(17) 1 d . . P A 12
S4 S 0.35016(2) 0.39933(5) 0.16053(4) 0.01263(12) Uani 0.9526(17) 1 d . . P B 14
Si1 Si 0.16017(3) 0.03766(6) 0.02881(4) 0.01151(9) Uani 1 1 d . . . . .
Se1 Se 0.06558(2) 0.15962(4) 0.54266(3) 0.01447(9) Uani 0.3988(18) 1 d . . P A 9
Se3 Se 0.21723(2) 0.43140(5) 0.41537(3) 0.01295(11) Uani 0.1215(17) 1 d . . P B
11
Se2 Se 0.14422(2) 0.24640(5) 0.14602(3) 0.01402(11) Uani 0.1266(17) 1 d . . P A
13
Se4 Se 0.35016(2) 0.39933(5) 0.16053(4) 0.01263(12) Uani 0.0474(17) 1 d . . P B
15
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Ce Ce -0.2486 2.6331 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.4742 1.8119 '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 Ce1 S3 135.148(7) 4_545 . ?
S3 Ce1 S3 70.373(11) 7_556 . ?
S2 Ce1 S2 125.155(10) 4_545 . ?
S2 Ce2 S2 132.546(15) 2 . ?
S1 Ce2 S1 162.156(11) 2 . ?
S4 Ce2 I1 121.993(8) 3_445 . ?
S4 Ce2 I1 121.993(8) 4_545 . ?
S2 Ce2 I1 66.273(8) 2 . ?
S2 Ce2 I1 66.273(8) . . ?
Se2 Ce2 I1 66.273(8) . . ?
S1 Ce2 I1 81.078(6) 2 . ?
S1 Ce2 I1 81.078(6) . . ?
Se1 Ce2 I1 81.078(6) . . ?
I1 Ce2 S1 127.501(5) . 6 ?
I1 Ce2 S1 127.501(5) . 5_556 ?
Ce2 I1 Ce1 104.023(3) . 4 ?
Ce2 I1 Ce1 104.023(3) . 3_455 ?
Ce1 I1 Ce1 151.955(7) 4 3_455 ?
Si1 S1 Ce1 89.652(15) 6_556 7_556 ?
Si1 S1 Ce2 87.655(15) 6_556 . ?
Ce1 S1 Ce2 134.498(10) 7_556 . ?
Si1 S1 Ce2 84.375(15) 6_556 5_556 ?
Ce1 S1 Ce2 105.865(9) 7_556 5_556 ?
Ce2 S1 Ce2 119.009(8) . 5_556 ?
Si1 S3 Ce1 91.987(17) 4 4 ?
Si1 S3 Ce1 89.128(17) 4 7_556 ?
Ce1 S3 Ce1 154.330(14) 4 7_556 ?
Si1 S3 Ce1 88.811(17) 4 . ?
Ce1 S3 Ce1 96.038(10) 4 . ?
Ce1 S3 Ce1 109.627(11) 7_556 . ?
Si1 S2 Ce2 94.708(18) . . ?
Si1 S2 Ce1 139.89(2) . 4 ?
Ce2 S2 Ce1 123.813(12) . 4 ?
Si1 S2 Ce1 87.838(18) . . ?
Ce2 S2 Ce1 104.801(11) . . ?
Ce1 S2 Ce1 92.073(10) 4 . ?
Si1 S4 Ce2 99.075(19) 7 3 ?
Si1 S4 Ce1 138.69(2) 7 . ?
Ce2 S4 Ce1 117.894(13) 3 . ?
Si1 S4 Ce1 88.915(18) 7 4 ?
Ce2 S4 Ce1 107.820(13) 3 4 ?
Ce1 S4 Ce1 96.119(11) . 4 ?
Si1 Se1 Ce1 89.652(15) 6_556 7_556 ?
Si1 Se1 Ce2 87.655(15) 6_556 . ?
Ce1 Se1 Ce2 134.498(10) 7_556 . ?
Si1 Se1 Ce2 84.375(15) 6_556 5_556 ?
Ce1 Se1 Ce2 105.865(9) 7_556 5_556 ?
Ce2 Se1 Ce2 119.009(8) . 5_556 ?
Si1 Se3 Ce1 91.987(17) 4 4 ?
Si1 Se3 Ce1 89.128(17) 4 7_556 ?
Ce1 Se3 Ce1 154.330(14) 4 7_556 ?
Si1 Se3 Ce1 88.811(17) 4 . ?
Ce1 Se3 Ce1 96.038(10) 4 . ?
Ce1 Se3 Ce1 109.627(11) 7_556 . ?
Si1 Se2 Ce2 94.708(18) . . ?
Si1 Se2 Ce1 139.89(2) . 4 ?
Ce2 Se2 Ce1 123.813(12) . 4 ?
Si1 Se2 Ce1 87.838(18) . . ?
Ce2 Se2 Ce1 104.801(11) . . ?
Ce1 Se2 Ce1 92.073(10) 4 . ?
Si1 Se4 Ce2 99.075(19) 7 3 ?
Si1 Se4 Ce1 138.69(2) 7 . ?
Ce2 Se4 Ce1 117.894(13) 3 . ?
Si1 Se4 Ce1 88.915(18) 7 4 ?
Ce2 Se4 Ce1 107.820(13) 3 4 ?
Ce1 Se4 Ce1 96.119(11) . 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
Ce1 S3 2.9342(4) 4_545 ?
Ce1 Se4 2.9608(4) . ?
Ce1 S4 2.9608(4) . ?
Ce1 S3 2.9996(4) 7_556 ?
Ce1 S1 3.0043(3) 7_556 ?
Ce1 S4 3.0361(4) 4_545 ?
Ce1 S3 3.0659(4) . ?
Ce1 Se3 3.0659(4) . ?
Ce1 S2 3.0868(4) 4_545 ?
Ce1 S2 3.1110(4) . ?
Ce1 Se2 3.1110(4) . ?
Ce1 I1 3.46822(12) 3_545 ?
Ce2 S4 2.9203(4) 3_445 ?
Ce2 S4 2.9203(4) 4_545 ?
Ce2 S2 2.9638(4) 2 ?
Ce2 S2 2.9638(4) . ?
Ce2 Se2 2.9638(4) . ?
Ce2 S1 3.2725(3) 2 ?
Ce2 S1 3.2725(3) . ?
Ce2 Se1 3.2725(3) . ?
Ce2 I1 3.3036(2) . ?
Ce2 S1 3.3058(3) 6 ?
Ce2 S1 3.3058(3) 5_556 ?
S1 Si1 2.1956(6) 6_556 ?
S3 Si1 2.1543(6) 4 ?
S2 Si1 2.1235(6) . ?
S4 Si1 2.1135(6) 7 ?
Si1 Se2 2.1235(6) . ?
