# Electronic Supplementary Material (ESI) for CrystEngComm.
# This journal is © The Royal Society of Chemistry 2020

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_Ce07
_database_code_depnum_ccdc_archive 'CCDC 2038458'
loop_
_audit_author_name
_audit_author_address
'Vladislav Klepov'
;University of South Carolina
United States of America
;
_audit_update_record             
;
2020-10-14 deposited with the CCDC.	2020-12-01 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/1
_shelx_SHELXL_version_number     2018/1
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'Ca0.30 Ce0.70 Cs0.30 P S4'
_chemical_formula_weight         309.19

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Ca Ca 0.2262 0.3064 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cs Cs -0.3680 2.1192 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ce Ce -0.2486 2.6331 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 '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'

_space_group_crystal_system      trigonal
_space_group_IT_number           166
_space_group_name_H-M_alt        'R -3 m :H'
_space_group_name_Hall           '-R 3 2"'

_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.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'y, x, -z'
'x-y, -y, -z'
'-x, -x+y, -z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'y+2/3, x+1/3, -z+1/3'
'x-y+2/3, -y+1/3, -z+1/3'
'-x+2/3, -x+y+1/3, -z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'y+1/3, x+2/3, -z+2/3'
'x-y+1/3, -y+2/3, -z+2/3'
'-x+1/3, -x+y+2/3, -z+2/3'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-y, -x, z'
'-x+y, y, z'
'x, x-y, z'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-y+2/3, -x+1/3, z+1/3'
'-x+y+2/3, y+1/3, z+1/3'
'x+2/3, x-y+1/3, z+1/3'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'
'-y+1/3, -x+2/3, z+2/3'
'-x+y+1/3, y+2/3, z+2/3'
'x+1/3, x-y+2/3, z+2/3'

_cell_length_a                   16.5183(3)
_cell_length_b                   16.5183(3)
_cell_length_c                   13.6408(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     3223.30(14)
_cell_formula_units_Z            18
_cell_measurement_temperature    300(2)
_cell_measurement_reflns_used    9698
_cell_measurement_theta_min      3.22
_cell_measurement_theta_max      36.23

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.867
_exptl_crystal_F_000             2558
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.060
_exptl_crystal_size_mid          0.060
_exptl_crystal_size_min          0.050
_exptl_absorpt_coefficient_mu    7.477
_shelx_estimated_absorpt_T_min   0.663
_shelx_estimated_absorpt_T_max   0.706
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.2214
_exptl_absorpt_correction_T_max  0.2740
_exptl_absorpt_process_details   
;
 Reference: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D.,
 J. Appl. Cryst. 48 (2015) 3-10.
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      300(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker D8 QUEST'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            37202
_diffrn_reflns_av_unetI/netI     0.0063
_diffrn_reflns_av_R_equivalents  0.0248
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         3.216
_diffrn_reflns_theta_max         27.439
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measured_fraction_theta_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_point_group_measured_fraction_full 0.990
_reflns_number_total             908
_reflns_number_gt                899
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2018/1 (Sheldrick, 2018)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0596P)²+66.6555P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   .
_refine_ls_hydrogen_treatment    undef
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         908
_refine_ls_number_parameters     43
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0388
_refine_ls_R_factor_gt           0.0387
_refine_ls_wR_factor_ref         0.1095
_refine_ls_wR_factor_gt          0.1094
_refine_ls_goodness_of_fit_ref   1.138
_refine_ls_restrained_S_all      1.138
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.001

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 0.000000 0.64515(3) 0.000000 0.0220(2) Uani 0.7 2 d S T P . .
Ca1 Ca 0.000000 0.64515(3) 0.000000 0.0220(2) Uani 0.3 2 d S T P . .
S1 S 0.19204(9) 0.80796(9) 0.00340(13) 0.0355(5) Uani 1 2 d S T P . .
S2 S -0.01912(10) 0.76423(11) -0.14893(10) 0.0312(3) Uani 1 1 d . . . . .
P1 P 0.15963(9) 0.84037(9) 0.13634(13) 0.0291(5) Uani 1 2 d S T P . .
S3 S 0.08769(15) 0.54384(8) 0.09049(15) 0.0309(5) Uani 1 2 d S T P . .
Cs1 Cs 0.333333 0.666667 0.166667 0.211(6) Uani 0.760(11) 12 d S T P . .
Cs2 Cs 0.000000 1.000000 0.000000 0.324(10) Uani 0.737(15) 12 d S T P . .
Cs3 Cs 0.000000 1.000000 -0.248(3) 0.24(2) Uani 0.152(7) 6 d S T P . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

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 S2 2.9524(14) . ?
Ce1 S2 2.9525(14) 6 ?
Ce1 S1 2.9608(4) . ?
Ce1 S1 2.9608(4) 20_455 ?
Ce1 S3 2.9742(12) . ?
Ce1 S3 2.9742(12) 19_565 ?
Ce1 S2 2.9770(14) 16_454 ?
Ce1 S2 2.9770(14) 8_565 ?
S1 P1 2.037(3) . ?
S2 P1 2.029(2) 20_455 ?
S2 Cs3 3.981(16) . ?
P1 S3 2.057(3) 26_455 ?
S3 Cs1 3.664(2) . ?
Cs1 Cs3 3.44(5) 13_545 ?
Cs1 Cs3 3.44(5) 31_564 ?
Cs2 Cs3 3.38(5) 19_575 ?
Cs2 Cs3 3.38(5) . ?

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
S2 Ce1 S2 87.94(6) . 6 ?
S2 Ce1 S1 80.13(6) . . ?
S2 Ce1 S1 68.60(5) 6 . ?
S2 Ce1 S1 68.60(5) . 20_455 ?
S2 Ce1 S1 80.12(6) 6 20_455 ?
S1 Ce1 S1 136.24(10) . 20_455 ?
S2 Ce1 S3 154.80(5) . . ?
S2 Ce1 S3 104.81(4) 6 . ?
S1 Ce1 S3 84.41(6) . . ?
S1 Ce1 S3 134.29(6) 20_455 . ?
S2 Ce1 S3 104.81(4) . 19_565 ?
S2 Ce1 S3 154.80(5) 6 19_565 ?
S1 Ce1 S3 134.29(6) . 19_565 ?
S1 Ce1 S3 84.41(6) 20_455 19_565 ?
S3 Ce1 S3 72.56(6) . 19_565 ?
S2 Ce1 S2 69.34(5) . 16_454 ?
S2 Ce1 S2 136.32(2) 6 16_454 ?
S1 Ce1 S2 70.98(4) . 16_454 ?
S1 Ce1 S2 121.17(5) 20_455 16_454 ?
S3 Ce1 S2 86.88(5) . 16_454 ?
S3 Ce1 S2 68.87(5) 19_565 16_454 ?
S2 Ce1 S2 136.32(2) . 8_565 ?
S2 Ce1 S2 69.34(5) 6 8_565 ?
S1 Ce1 S2 121.17(5) . 8_565 ?
S1 Ce1 S2 70.98(4) 20_455 8_565 ?
S3 Ce1 S2 68.87(5) . 8_565 ?
S3 Ce1 S2 86.88(5) 19_565 8_565 ?
S2 Ce1 S2 150.17(6) 16_454 8_565 ?
P1 S1 Ce1 87.12(4) . . ?
P1 S1 Ce1 87.12(4) . 21_665 ?
Ce1 S1 Ce1 163.67(11) . 21_665 ?
P1 S2 Ce1 87.48(7) 20_455 . ?
P1 S2 Ce1 90.14(8) 20_455 15_454 ?
Ce1 S2 Ce1 101.40(4) . 15_454 ?
P1 S2 Cs3 101.40(7) 20_455 . ?
Ce1 S2 Cs3 154.4(6) . . ?
Ce1 S2 Cs3 102.5(6) 15_454 . ?
S2 P1 S2 107.03(14) 21_665 6 ?
S2 P1 S1 110.08(8) 21_665 . ?
S2 P1 S1 110.08(8) 6 . ?
S2 P1 S3 110.91(8) 21_665 26_455 ?
S2 P1 S3 110.91(8) 6 26_455 ?
S1 P1 S3 107.86(14) . 26_455 ?
P1 S3 Ce1 89.69(6) 27 19_565 ?
P1 S3 Ce1 89.69(6) 27 . ?
Ce1 S3 Ce1 107.44(6) 19_565 . ?
P1 S3 Cs1 118.59(9) 27 . ?
Ce1 S3 Cs1 121.48(4) 19_565 . ?
Ce1 S3 Cs1 121.48(4) . . ?
Cs3 Cs1 Cs3 180.0 13_545 31_564 ?
Cs3 Cs1 S3 73.53(3) 13_545 25_565 ?
Cs3 Cs1 S3 106.47(3) 31_564 25_565 ?
Cs3 Cs1 S3 73.53(3) 13_545 27 ?
Cs3 Cs1 S3 106.47(3) 31_564 27 ?
S3 Cs1 S3 112.30(3) 25_565 27 ?
Cs3 Cs1 S3 106.47(3) 13_545 3_565 ?
Cs3 Cs1 S3 73.53(3) 31_564 3_565 ?
S3 Cs1 S3 67.70(3) 25_565 3_565 ?
S3 Cs1 S3 180.0 27 3_565 ?
Cs3 Cs1 S3 106.47(3) 13_545 2_665 ?
Cs3 Cs1 S3 73.53(3) 31_564 2_665 ?
S3 Cs1 S3 67.71(3) 25_565 2_665 ?
S3 Cs1 S3 67.71(3) 27 2_665 ?
S3 Cs1 S3 112.30(3) 3_565 2_665 ?
Cs3 Cs1 S3 106.47(3) 13_545 . ?
Cs3 Cs1 S3 73.53(3) 31_564 . ?
S3 Cs1 S3 180.0 25_565 . ?
S3 Cs1 S3 67.70(3) 27 . ?
S3 Cs1 S3 112.30(3) 3_565 . ?
S3 Cs1 S3 112.30(3) 2_665 . ?
Cs3 Cs1 S3 73.53(3) 13_545 26_455 ?
Cs3 Cs1 S3 106.47(3) 31_564 26_455 ?
S3 Cs1 S3 112.29(3) 25_565 26_455 ?
S3 Cs1 S3 112.29(3) 27 26_455 ?
S3 Cs1 S3 67.70(3) 3_565 26_455 ?
S3 Cs1 S3 180.0 2_665 26_455 ?
S3 Cs1 S3 67.70(3) . 26_455 ?
Cs3 Cs2 Cs3 180.0 19_575 . ?
Cs2 Cs3 Cs1 180.0 . 7_454 ?
Cs2 Cs3 S2 70.2(6) . 24_575 ?
Cs1 Cs3 S2 109.8(6) 7_454 24_575 ?
Cs2 Cs3 S2 70.2(6) . 3_465 ?
Cs1 Cs3 S2 109.8(6) 7_454 3_465 ?
S2 Cs3 S2 48.4(2) 24_575 3_465 ?
Cs2 Cs3 S2 70.3(6) . . ?
Cs1 Cs3 S2 109.7(6) 7_454 . ?
S2 Cs3 S2 139.7(12) 24_575 . ?
S2 Cs3 S2 109.2(6) 3_465 . ?
Cs2 Cs3 S2 70.2(6) . 2_675 ?
Cs1 Cs3 S2 109.8(6) 7_454 2_675 ?
S2 Cs3 S2 63.9(3) 24_575 2_675 ?
S2 Cs3 S2 109.2(6) 3_465 2_675 ?
S2 Cs3 S2 109.2(6) . 2_675 ?
Cs2 Cs3 S2 70.2(6) . 23_455 ?
Cs1 Cs3 S2 109.8(6) 7_454 23_455 ?
S2 Cs3 S2 109.2(6) 24_575 23_455 ?
S2 Cs3 S2 63.9(3) 3_465 23_455 ?
S2 Cs3 S2 48.4(2) . 23_455 ?
S2 Cs3 S2 139.7(12) 2_675 23_455 ?
Cs2 Cs3 S2 70.3(6) . 22_665 ?
Cs1 Cs3 S2 109.7(6) 7_454 22_665 ?
S2 Cs3 S2 109.2(6) 24_575 22_665 ?
S2 Cs3 S2 139.7(12) 3_465 22_665 ?
S2 Cs3 S2 63.9(3) . 22_665 ?
S2 Cs3 S2 48.4(2) 2_675 22_665 ?
S2 Cs3 S2 109.2(6) 23_455 22_665 ?

_refine_diff_density_max         3.741
_refine_diff_density_min         -3.951
_refine_diff_density_rms         0.227



# start Validation Reply Form
_vrf_PLAT971_1                   
;
PROBLEM: Check Calcd Resid. Dens.  1.07A   From Cs2             3.83 eA-3  
RESPONSE: The cesium atoms are severely disordered along the
channels in the structure and cannot be located from the difference map.
Due to this they have been resolved as residing at three positions with
overall occupancy equal to 0.15 to accomplish charge balance.
;
_vrf_PLAT974_1                   
;
PROBLEM: Check Calcd Negative Resid. Density on       Cs2      -4.07 eA-3  
RESPONSE: The cesium atoms are severely disordered along the
channels in the structure and cannot be located from the difference map.
Due to this they have been resolved as residing at three positions with
overall occupancy equal to 0.15 to accomplish charge balance.
;
_vrf_PLAT260_1                   
;
PROBLEM: Large Average Ueq of Residue Including       Cs2      0.323 Check 
RESPONSE: The cesium atoms are severely disordered along the
channels in the structure and cannot be located from the difference map.
Due to this they have been resolved as residing at three positions with
overall occupancy equal to 0.15 to accomplish charge balance.
;
_vrf_PLAT973_1                   
;
PROBLEM: Check Calcd Positive Resid. Density on       Cs1       1.64 eA-3  
RESPONSE: The cesium atoms are severely disordered along the
channels in the structure and cannot be located from the difference map.
Due to this they have been resolved as residing at three positions with
overall occupancy equal to 0.15 to accomplish charge balance.
;
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_Pr05
_database_code_depnum_ccdc_archive 'CCDC 2038465'
loop_
_audit_author_name
_audit_author_address
'Vladislav Klepov'
;University of South Carolina
United States of America
;
_audit_update_record             
;
2020-10-14 deposited with the CCDC.	2020-12-01 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/1
_shelx_SHELXL_version_number     2018/1
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'Ca0.50 Cs0.50 P Pr0.50 S4'
_chemical_formula_weight         316.16

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
P P 0.1023 0.0942 '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'
Ca Ca 0.2262 0.3064 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cs Cs -0.3680 2.1192 '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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 2/c'
_space_group_name_Hall           '-C 2yc'

_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.
;

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'

_cell_length_a                   9.2095(2)
_cell_length_b                   9.2341(2)
_cell_length_c                   16.7221(4)
_cell_angle_alpha                90
_cell_angle_beta                 103.9463(8)
_cell_angle_gamma                90
_cell_volume                     1380.15(5)
_cell_formula_units_Z            8
_cell_measurement_temperature    300(2)
_cell_measurement_reflns_used    9982
_cell_measurement_theta_min      2.51
_cell_measurement_theta_max      33.15

_exptl_crystal_description       plate
_exptl_crystal_colour            'pale green'
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    3.043
_exptl_crystal_F_000             1168
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.04
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.01
_exptl_absorpt_coefficient_mu    7.897
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.1994
_exptl_absorpt_correction_T_max  0.2694
_exptl_absorpt_process_details   
;
 Reference: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D.,
 J. Appl. Cryst. 48 (2015) 3-10.
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      300(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker D8 QUEST'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            26261
_diffrn_reflns_av_unetI/netI     0.0148
_diffrn_reflns_av_R_equivalents  0.0313
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_theta_min         3.172
_diffrn_reflns_theta_max         32.487
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.996
_reflns_number_total             2487
_reflns_number_gt                2338
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2018/1 (Sheldrick, 2018)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0215P)²+8.4284P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   .
_refine_ls_hydrogen_treatment    undef
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         2487
_refine_ls_number_parameters     60
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0287
_refine_ls_R_factor_gt           0.0267
_refine_ls_wR_factor_ref         0.0642
_refine_ls_wR_factor_gt          0.0631
_refine_ls_goodness_of_fit_ref   1.116
_refine_ls_restrained_S_all      1.116
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

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
Cs1 Cs 0.000000 0.64236(3) 0.250000 0.03376(8) Uani 1 2 d S T P . .
Pr1 Pr 0.49342(3) 0.73185(3) 0.02453(2) 0.02494(7) Uani 0.5 1 d . . P . .
Ca1 Ca 0.49342(3) 0.73185(3) 0.02453(2) 0.02494(7) Uani 0.5 1 d . . P . .
P1 P 0.27645(8) 0.48573(7) 0.09301(4) 0.01996(13) Uani 1 1 d . . . . .
S1 S 0.25343(9) 0.70130(8) 0.11300(5) 0.02676(14) Uani 1 1 d . . . . .
S2 S 0.18326(8) 0.36098(8) 0.16604(5) 0.02473(13) Uani 1 1 d . . . . .
S3 S 0.50129(8) 0.45422(8) 0.11325(5) 0.02726(15) Uani 1 1 d . . . . .
S4 S 0.18214(12) 0.44405(12) -0.02911(5) 0.0437(2) Uani 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

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
Cs1 S2 3.5470(8) 4 ?
Cs1 S2 3.5470(8) 3_455 ?
Cs1 S2 3.5656(8) 2 ?
Cs1 S2 3.5656(8) . ?
Cs1 S3 3.6790(8) 4 ?
Cs1 S3 3.6790(8) 3_455 ?
Cs1 S1 3.6837(8) 2 ?
Cs1 S1 3.6837(8) . ?
Cs1 S4 3.7561(9) 5_565 ?
Cs1 S4 3.7561(9) 6_566 ?
Cs1 Pr1 4.7499(3) 8_466 ?
Cs1 Pr1 4.7499(3) 7_565 ?
Ca1 S2 2.8431(8) 3 ?
Ca1 S3 2.8839(9) 5_665 ?
Ca1 S1 2.8841(8) 7_565 ?
Ca1 S4 2.9010(9) 3 ?
Ca1 S3 2.9541(8) . ?
Ca1 S1 2.9544(8) . ?
Ca1 S4 3.3855(13) 5_665 ?
Ca1 P1 3.4018(7) . ?
Ca1 S4 3.4112(13) 7_565 ?
Ca1 P1 3.4875(7) 3 ?
P1 S2 2.0150(10) . ?
P1 S3 2.0369(10) . ?
P1 S1 2.0379(10) . ?
P1 S4 2.0537(11) . ?

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
S2 Cs1 S2 110.62(3) 4 3_455 ?
S2 Cs1 S2 132.92(2) 4 2 ?
S2 Cs1 S2 98.537(9) 3_455 2 ?
S2 Cs1 S2 98.537(9) 4 . ?
S2 Cs1 S2 132.92(2) 3_455 . ?
S2 Cs1 S2 86.44(2) 2 . ?
S2 Cs1 S3 55.531(16) 4 4 ?
S2 Cs1 S3 71.035(18) 3_455 4 ?
S2 Cs1 S3 104.650(16) 2 4 ?
S2 Cs1 S3 152.611(17) . 4 ?
S2 Cs1 S3 71.035(18) 4 3_455 ?
S2 Cs1 S3 55.531(16) 3_455 3_455 ?
S2 Cs1 S3 152.611(17) 2 3_455 ?
S2 Cs1 S3 104.649(16) . 3_455 ?
S3 Cs1 S3 76.98(3) 4 3_455 ?
S2 Cs1 S1 104.693(17) 4 2 ?
S2 Cs1 S1 65.052(17) 3_455 2 ?
S2 Cs1 S1 55.374(16) 2 2 ?
S2 Cs1 S1 141.586(18) . 2 ?
S3 Cs1 S1 53.155(16) 4 2 ?
S3 Cs1 S1 111.615(17) 3_455 2 ?
S2 Cs1 S1 65.052(17) 4 . ?
S2 Cs1 S1 104.693(17) 3_455 . ?
S2 Cs1 S1 141.586(18) 2 . ?
S2 Cs1 S1 55.374(16) . . ?
S3 Cs1 S1 111.615(18) 4 . ?
S3 Cs1 S1 53.155(16) 3_455 . ?
S1 Cs1 S1 163.01(2) 2 . ?
S2 Cs1 S4 129.785(18) 4 5_565 ?
S2 Cs1 S4 66.54(2) 3_455 5_565 ?
S2 Cs1 S4 95.213(19) 2 5_565 ?
S2 Cs1 S4 66.39(2) . 5_565 ?
S3 Cs1 S4 135.23(2) 4 5_565 ?
S3 Cs1 S4 67.83(2) 3_455 5_565 ?
S1 Cs1 S4 116.31(2) 2 5_565 ?
S1 Cs1 S4 67.63(2) . 5_565 ?
S2 Cs1 S4 66.54(2) 4 6_566 ?
S2 Cs1 S4 129.785(18) 3_455 6_566 ?
S2 Cs1 S4 66.39(2) 2 6_566 ?
S2 Cs1 S4 95.214(18) . 6_566 ?
S3 Cs1 S4 67.83(2) 4 6_566 ?
S3 Cs1 S4 135.23(2) 3_455 6_566 ?
S1 Cs1 S4 67.64(2) 2 6_566 ?
S1 Cs1 S4 116.31(2) . 6_566 ?
S4 Cs1 S4 155.47(4) 5_565 6_566 ?
S2 Cs1 Pr1 71.282(12) 4 8_466 ?
S2 Cs1 Pr1 92.439(13) 3_455 8_466 ?
S2 Cs1 Pr1 71.345(12) 2 8_466 ?
S2 Cs1 Pr1 132.554(13) . 8_466 ?
S3 Cs1 Pr1 37.359(13) 4 8_466 ?
S3 Cs1 Pr1 114.333(15) 3_455 8_466 ?
S1 Cs1 Pr1 37.365(13) 2 8_466 ?
S1 Cs1 Pr1 136.263(14) . 8_466 ?
S4 Cs1 Pr1 153.601(18) 5_565 8_466 ?
S4 Cs1 Pr1 37.644(13) 6_566 8_466 ?
S2 Cs1 Pr1 92.439(13) 4 7_565 ?
S2 Cs1 Pr1 71.282(12) 3_455 7_565 ?
S2 Cs1 Pr1 132.554(13) 2 7_565 ?
S2 Cs1 Pr1 71.344(12) . 7_565 ?
S3 Cs1 Pr1 114.333(15) 4 7_565 ?
S3 Cs1 Pr1 37.359(13) 3_455 7_565 ?
S1 Cs1 Pr1 136.263(14) 2 7_565 ?
S1 Cs1 Pr1 37.365(13) . 7_565 ?
S4 Cs1 Pr1 37.644(13) 5_565 7_565 ?
S4 Cs1 Pr1 153.601(18) 6_566 7_565 ?
Pr1 Cs1 Pr1 151.691(10) 8_466 7_565 ?
S2 Ca1 S3 142.13(2) 3 5_665 ?
S2 Ca1 S1 141.47(2) 3 7_565 ?
S3 Ca1 S1 69.65(2) 5_665 7_565 ?
S2 Ca1 S4 71.34(2) 3 3 ?
S3 Ca1 S4 91.64(3) 5_665 3 ?
S1 Ca1 S4 91.42(3) 7_565 3 ?
S2 Ca1 S3 90.59(2) 3 . ?
S3 Ca1 S3 83.17(2) 5_665 . ?
S1 Ca1 S3 120.36(2) 7_565 . ?
S4 Ca1 S3 142.88(3) 3 . ?
S2 Ca1 S1 90.43(2) 3 . ?
S3 Ca1 S1 120.12(2) 5_665 . ?
S1 Ca1 S1 83.03(2) 7_565 . ?
S4 Ca1 S1 142.70(3) 3 . ?
S3 Ca1 S1 66.20(2) . . ?
S2 Ca1 S4 79.63(2) 3 5_665 ?
S3 Ca1 S4 63.09(2) 5_665 5_665 ?
S1 Ca1 S4 129.98(2) 7_565 5_665 ?
S4 Ca1 S4 74.92(4) 3 5_665 ?
S3 Ca1 S4 69.98(2) . 5_665 ?
S1 Ca1 S4 134.87(2) . 5_665 ?
S2 Ca1 P1 107.05(2) 3 . ?
S3 Ca1 P1 89.73(2) 5_665 . ?
S1 Ca1 P1 89.85(2) 7_565 . ?
S4 Ca1 P1 178.39(2) 3 . ?
S3 Ca1 P1 36.531(18) . . ?
S1 Ca1 P1 36.551(18) . . ?
S4 Ca1 P1 104.99(2) 5_665 . ?
S2 Ca1 S4 79.23(2) 3 7_565 ?
S3 Ca1 S4 129.79(2) 5_665 7_565 ?
S1 Ca1 S4 62.83(2) 7_565 7_565 ?
S4 Ca1 S4 74.74(3) 3 7_565 ?
S3 Ca1 S4 134.79(2) . 7_565 ?
S1 Ca1 S4 69.92(2) . 7_565 ?
S4 Ca1 S4 147.24(3) 5_665 7_565 ?
P1 Ca1 S4 104.98(2) . 7_565 ?
S2 Ca1 P1 35.294(18) 3 3 ?
S3 Ca1 P1 120.50(2) 5_665 3 ?
S1 Ca1 P1 120.07(2) 7_565 3 ?
S4 Ca1 P1 36.04(2) 3 3 ?
S3 Ca1 P1 119.51(2) . 3 ?
S1 Ca1 P1 119.33(2) . 3 ?
S4 Ca1 P1 74.30(2) 5_665 3 ?
P1 Ca1 P1 142.35(2) . 3 ?
S4 Ca1 P1 73.96(2) 7_565 3 ?
S2 Ca1 Cs1 123.595(16) 3 7_565 ?
S3 Ca1 Cs1 50.724(16) 5_665 7_565 ?
S1 Ca1 Cs1 50.817(15) 7_565 7_565 ?
S4 Ca1 Cs1 52.257(18) 3 7_565 ?
S3 Ca1 Cs1 133.875(18) . 7_565 ?
S1 Ca1 Cs1 133.838(17) . 7_565 ?
S4 Ca1 Cs1 85.549(15) 5_665 7_565 ?
P1 Ca1 Cs1 129.351(14) . 7_565 ?
S4 Ca1 Cs1 85.622(15) 7_565 7_565 ?
P1 Ca1 Cs1 88.301(13) 3 7_565 ?
S2 P1 S3 112.46(5) . . ?
S2 P1 S1 112.50(4) . . ?
S3 P1 S1 104.72(4) . . ?
S2 P1 S4 110.83(5) . . ?
S3 P1 S4 107.93(5) . . ?
S1 P1 S4 108.08(5) . . ?
S2 P1 Ca1 163.04(4) . . ?
S3 P1 Ca1 59.69(3) . . ?
S1 P1 Ca1 59.70(3) . . ?
S4 P1 Ca1 86.13(3) . . ?
P1 S1 Pr1 99.87(4) . 7_565 ?
P1 S1 Ca1 83.75(3) . . ?
Pr1 S1 Ca1 96.97(2) 7_565 . ?
P1 S1 Cs1 93.68(3) . . ?
Pr1 S1 Cs1 91.82(2) 7_565 . ?
Ca1 S1 Cs1 171.14(3) . . ?
P1 S2 Pr1 90.10(3) . 3_445 ?
P1 S2 Cs1 97.79(3) . 3_545 ?
Pr1 S2 Cs1 111.89(2) 3_445 3_545 ?
P1 S2 Cs1 97.65(3) . . ?
Pr1 S2 Cs1 112.26(2) 3_445 . ?
Cs1 S2 Cs1 132.92(2) 3_545 . ?
P1 S3 Pr1 99.48(4) . 5_665 ?
P1 S3 Ca1 83.78(3) . . ?
Pr1 S3 Ca1 96.83(2) 5_665 . ?
P1 S3 Cs1 93.42(3) . 3_545 ?
Pr1 S3 Cs1 91.92(2) 5_665 3_545 ?
Ca1 S3 Cs1 171.14(3) . 3_545 ?
P1 S4 Pr1 87.74(3) . 3_445 ?
P1 S4 Cs1 177.84(4) . 5_565 ?
Pr1 S4 Cs1 90.10(2) 3_445 5_565 ?

_refine_diff_density_max         1.190
_refine_diff_density_min         -1.057
_refine_diff_density_rms         0.127

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_Sm07
_database_code_depnum_ccdc_archive 'CCDC 2038461'
loop_
_audit_author_name
_audit_author_address
'Vladislav Klepov'
;University of South Carolina
United States of America
;
_audit_update_record             
;
2020-10-14 deposited with the CCDC.	2020-12-01 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/1
_shelx_SHELXL_version_number     2018/1
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'Ca0.30 Cs0.30 P S4 Sm0.70'
_chemical_formula_weight         316.35

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Ca Ca 0.2262 0.3064 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cs Cs -0.3680 2.1192 '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'
P P 0.1023 0.0942 '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'

_space_group_crystal_system      trigonal
_space_group_IT_number           166
_space_group_name_H-M_alt        'R -3 m :H'
_space_group_name_Hall           '-R 3 2"'

_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.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'y, x, -z'
'x-y, -y, -z'
'-x, -x+y, -z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'y+2/3, x+1/3, -z+1/3'
'x-y+2/3, -y+1/3, -z+1/3'
'-x+2/3, -x+y+1/3, -z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'y+1/3, x+2/3, -z+2/3'
'x-y+1/3, -y+2/3, -z+2/3'
'-x+1/3, -x+y+2/3, -z+2/3'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-y, -x, z'
'-x+y, y, z'
'x, x-y, z'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-y+2/3, -x+1/3, z+1/3'
'-x+y+2/3, y+1/3, z+1/3'
'x+2/3, x-y+1/3, z+1/3'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'
'-y+1/3, -x+2/3, z+2/3'
'-x+y+1/3, y+2/3, z+2/3'
'x+1/3, x-y+2/3, z+2/3'

_cell_length_a                   16.4128(3)
_cell_length_b                   16.4128(3)
_cell_length_c                   13.4526(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     3138.35(13)
_cell_formula_units_Z            18
_cell_measurement_temperature    300(2)
_cell_measurement_reflns_used    9909
_cell_measurement_theta_min      2.48
_cell_measurement_theta_max      30.52

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    3.013
_exptl_crystal_F_000             2608
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.050
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.030
_exptl_absorpt_coefficient_mu    9.004
_shelx_estimated_absorpt_T_min   0.662
_shelx_estimated_absorpt_T_max   0.774
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.1221
_exptl_absorpt_correction_T_max  0.1561
_exptl_absorpt_process_details   
;
 Reference: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D.,
 J. Appl. Cryst. 48 (2015) 3-10.
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      300(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker D8 QUEST'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            30331
_diffrn_reflns_av_unetI/netI     0.0087
_diffrn_reflns_av_R_equivalents  0.0274
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         3.242
_diffrn_reflns_theta_max         29.994
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measured_fraction_theta_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_point_group_measured_fraction_full 0.994
_reflns_number_total             1124
_reflns_number_gt                1086
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2018/1 (Sheldrick, 2018)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0750P)²+48.3694P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   .
_refine_ls_hydrogen_treatment    undef
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         1124
_refine_ls_number_parameters     43
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0352
_refine_ls_R_factor_gt           0.0343
_refine_ls_wR_factor_ref         0.1075
_refine_ls_wR_factor_gt          0.1061
_refine_ls_goodness_of_fit_ref   0.980
_refine_ls_restrained_S_all      0.980
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

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
Sm1 Sm 0.000000 0.64459(2) 0.000000 0.02323(16) Uani 0.7 2 d S T P . .
Ca1 Ca 0.000000 0.64459(2) 0.000000 0.02323(16) Uani 0.3 2 d S T P . .
S1 S 0.19298(7) 0.80702(7) 0.00180(11) 0.0345(4) Uani 1 2 d S T P . .
S2 S -0.01938(8) 0.76260(9) -0.14849(8) 0.0319(3) Uani 1 1 d . . . . .
P1 P 0.16061(7) 0.83939(7) 0.13615(10) 0.0289(3) Uani 1 2 d S T P . .
S3 S 0.08876(12) 0.54438(6) 0.08830(12) 0.0318(3) Uani 1 2 d S T P . .
Cs1 Cs 0.333333 0.666667 0.166667 0.224(5) Uani 0.787(9) 12 d S T P . .
Cs2 Cs 0.000000 1.000000 0.000000 0.277(8) Uani 0.662(12) 12 d S T P . .
Cs3 Cs 0.000000 1.000000 -0.233(2) 0.186(12) Uani 0.176(6) 6 d S T P . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

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
Sm1 S2 2.9085(12) 6 ?
Sm1 S2 2.9085(12) . ?
Sm1 S2 2.9318(12) 8_565 ?
Sm1 S2 2.9318(12) 16_454 ?
Sm1 S3 2.9384(10) . ?
Sm1 S3 2.9385(10) 19_565 ?
Sm1 S1 2.9489(3) . ?
Sm1 S1 2.9489(3) 20_455 ?
S1 P1 2.028(2) . ?
S2 P1 2.0259(16) 20_455 ?
S2 Cs3 3.914(8) . ?
P1 S3 2.050(3) 26_455 ?
S3 Cs1 3.6327(17) . ?
Cs1 Cs3 3.60(3) 13_545 ?
Cs1 Cs3 3.60(3) 31_564 ?
Cs2 Cs3 3.13(3) 19_575 ?
Cs2 Cs3 3.13(3) . ?

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
S2 Sm1 S2 87.79(5) 6 . ?
S2 Sm1 S2 69.16(4) 6 8_565 ?
S2 Sm1 S2 136.148(19) . 8_565 ?
S2 Sm1 S2 136.149(19) 6 16_454 ?
S2 Sm1 S2 69.16(4) . 16_454 ?
S2 Sm1 S2 150.63(5) 8_565 16_454 ?
S2 Sm1 S3 105.29(4) 6 . ?
S2 Sm1 S3 154.20(4) . . ?
S2 Sm1 S3 69.64(4) 8_565 . ?
S2 Sm1 S3 86.47(4) 16_454 . ?
S2 Sm1 S3 154.20(4) 6 19_565 ?
S2 Sm1 S3 105.29(4) . 19_565 ?
S2 Sm1 S3 86.47(4) 8_565 19_565 ?
S2 Sm1 S3 69.64(4) 16_454 19_565 ?
S3 Sm1 S3 72.27(5) . 19_565 ?
S2 Sm1 S1 69.01(4) 6 . ?
S2 Sm1 S1 80.17(4) . . ?
S2 Sm1 S1 121.25(4) 8_565 . ?
S2 Sm1 S1 70.57(4) 16_454 . ?
S3 Sm1 S1 83.90(5) . . ?
S3 Sm1 S1 134.35(5) 19_565 . ?
S2 Sm1 S1 80.17(4) 6 20_455 ?
S2 Sm1 S1 69.01(4) . 20_455 ?
S2 Sm1 S1 70.57(4) 8_565 20_455 ?
S2 Sm1 S1 121.25(4) 16_454 20_455 ?
S3 Sm1 S1 134.36(5) . 20_455 ?
S3 Sm1 S1 83.90(5) 19_565 20_455 ?
S1 Sm1 S1 136.94(8) . 20_455 ?
P1 S1 Sm1 86.59(3) . . ?
P1 S1 Sm1 86.59(3) . 21_665 ?
Sm1 S1 Sm1 163.04(8) . 21_665 ?
P1 S2 Sm1 87.73(5) 20_455 . ?
P1 S2 Sm1 90.00(6) 20_455 15_454 ?
Sm1 S2 Sm1 101.66(4) . 15_454 ?
P1 S2 Cs3 101.28(6) 20_455 . ?
Sm1 S2 Cs3 151.6(4) . . ?
Sm1 S2 Cs3 105.2(4) 15_454 . ?
S2 P1 S2 107.14(11) 21_665 6 ?
S2 P1 S1 109.87(7) 21_665 . ?
S2 P1 S1 109.87(7) 6 . ?
S2 P1 S3 110.66(6) 21_665 26_455 ?
S2 P1 S3 110.66(6) 6 26_455 ?
S1 P1 S3 108.64(11) . 26_455 ?
S2 P1 Ca1 55.36(4) 21_665 26_455 ?
S2 P1 Ca1 120.21(6) 6 26_455 ?
S1 P1 Ca1 129.91(5) . 26_455 ?
S3 P1 Ca1 55.54(4) 26_455 26_455 ?
S2 P1 Ca1 120.21(6) 21_665 8_565 ?
S2 P1 Ca1 55.36(4) 6 8_565 ?
S1 P1 Ca1 129.91(5) . 8_565 ?
S3 P1 Ca1 55.54(4) 26_455 8_565 ?
Ca1 P1 Ca1 83.51(3) 26_455 8_565 ?
P1 S3 Sm1 89.35(5) 27 19_565 ?
P1 S3 Sm1 89.34(5) 27 . ?
Sm1 S3 Sm1 107.73(5) 19_565 . ?
P1 S3 Cs1 117.51(7) 27 . ?
Sm1 S3 Cs1 121.88(3) 19_565 . ?
Sm1 S3 Cs1 121.88(3) . . ?
Cs3 Cs1 Cs3 180.0 13_545 31_564 ?
Cs3 Cs1 S3 106.87(3) 13_545 2_665 ?
Cs3 Cs1 S3 73.13(3) 31_564 2_665 ?
Cs3 Cs1 S3 106.87(3) 13_545 . ?
Cs3 Cs1 S3 73.13(3) 31_564 . ?
S3 Cs1 S3 111.94(2) 2_665 . ?
Cs3 Cs1 S3 73.13(3) 13_545 26_455 ?
Cs3 Cs1 S3 106.87(3) 31_564 26_455 ?
S3 Cs1 S3 180.0 2_665 26_455 ?
S3 Cs1 S3 68.06(2) . 26_455 ?
Cs3 Cs1 S3 73.13(3) 13_545 25_565 ?
Cs3 Cs1 S3 106.87(3) 31_564 25_565 ?
S3 Cs1 S3 68.06(2) 2_665 25_565 ?
S3 Cs1 S3 180.0 . 25_565 ?
S3 Cs1 S3 111.94(2) 26_455 25_565 ?
Cs3 Cs1 S3 73.13(3) 13_545 27 ?
Cs3 Cs1 S3 106.87(3) 31_564 27 ?
S3 Cs1 S3 68.06(2) 2_665 27 ?
S3 Cs1 S3 68.06(2) . 27 ?
S3 Cs1 S3 111.94(2) 26_455 27 ?
S3 Cs1 S3 111.94(2) 25_565 27 ?
Cs3 Cs1 S3 106.87(3) 13_545 3_565 ?
Cs3 Cs1 S3 73.13(3) 31_564 3_565 ?
S3 Cs1 S3 111.94(2) 2_665 3_565 ?
S3 Cs1 S3 111.94(2) . 3_565 ?
S3 Cs1 S3 68.06(2) 26_455 3_565 ?
S3 Cs1 S3 68.06(2) 25_565 3_565 ?
S3 Cs1 S3 180.0 27 3_565 ?
Cs3 Cs2 Cs3 180.0 19_575 . ?
Cs2 Cs3 Cs1 180.0 . 7_454 ?
Cs2 Cs3 S2 73.2(4) . 2_675 ?
Cs1 Cs3 S2 106.8(4) 7_454 2_675 ?
Cs2 Cs3 S2 73.2(4) . 23_455 ?
Cs1 Cs3 S2 106.8(4) 7_454 23_455 ?
S2 Cs3 S2 145.4(8) 2_675 23_455 ?
Cs2 Cs3 S2 73.2(4) . 22_665 ?
Cs1 Cs3 S2 106.8(4) 7_454 22_665 ?
S2 Cs3 S2 49.22(11) 2_675 22_665 ?
S2 Cs3 S2 112.0(4) 23_455 22_665 ?
Cs2 Cs3 S2 73.2(4) . 24_575 ?
Cs1 Cs3 S2 106.8(4) 7_454 24_575 ?
S2 Cs3 S2 65.14(16) 2_675 24_575 ?
S2 Cs3 S2 112.0(4) 23_455 24_575 ?
S2 Cs3 S2 112.0(4) 22_665 24_575 ?
Cs2 Cs3 S2 73.2(4) . 3_465 ?
Cs1 Cs3 S2 106.8(4) 7_454 3_465 ?
S2 Cs3 S2 112.0(4) 2_675 3_465 ?
S2 Cs3 S2 65.14(16) 23_455 3_465 ?
S2 Cs3 S2 145.4(8) 22_665 3_465 ?
S2 Cs3 S2 49.22(11) 24_575 3_465 ?
Cs2 Cs3 S2 73.2(4) . . ?
Cs1 Cs3 S2 106.8(4) 7_454 . ?
S2 Cs3 S2 112.0(4) 2_675 . ?
S2 Cs3 S2 49.22(11) 23_455 . ?
S2 Cs3 S2 65.14(16) 22_665 . ?
S2 Cs3 S2 145.4(8) 24_575 . ?
S2 Cs3 S2 112.0(4) 3_465 . ?

_refine_diff_density_max         3.484
_refine_diff_density_min         -3.564
_refine_diff_density_rms         0.233


# start Validation Reply Form
_vrf_PLAT974_1                   
;
PROBLEM: Check Calcd Negative Resid. Density on       Cs2      -3.60 eA-3  
RESPONSE: The cesium atoms are severely disordered along the
channels in the structure and cannot be located from the difference map.
Due to this they have been resolved as residing at three positions with
overall occupancy equal to 0.15 to accomplish charge balance.
;
_vrf_PLAT971_1                   
;
PROBLEM: Check Calcd Resid. Dens.  1.06A   From Cs2             3.49 eA-3  
RESPONSE: The cesium atoms are severely disordered along the
channels in the structure and cannot be located from the difference map.
Due to this they have been resolved as residing at three positions with
overall occupancy equal to 0.15 to accomplish charge balance.
;
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_Pr07
_database_code_depnum_ccdc_archive 'CCDC 2038459'
loop_
_audit_author_name
_audit_author_address
'Vladislav Klepov'
;University of South Carolina
United States of America
;
_audit_update_record             
;
2020-10-14 deposited with the CCDC.	2020-12-01 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/1
_shelx_SHELXL_version_number     2018/1
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'Ca0.30 Cs0.30 P Pr0.70 S4'
_chemical_formula_weight         309.74

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Ca Ca 0.2262 0.3064 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cs Cs -0.3680 2.1192 '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'
P P 0.1023 0.0942 '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'

_space_group_crystal_system      trigonal
_space_group_IT_number           166
_space_group_name_H-M_alt        'R -3 m :H'
_space_group_name_Hall           '-R 3 2"'

_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.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'y, x, -z'
'x-y, -y, -z'
'-x, -x+y, -z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'y+2/3, x+1/3, -z+1/3'
'x-y+2/3, -y+1/3, -z+1/3'
'-x+2/3, -x+y+1/3, -z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'y+1/3, x+2/3, -z+2/3'
'x-y+1/3, -y+2/3, -z+2/3'
'-x+1/3, -x+y+2/3, -z+2/3'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-y, -x, z'
'-x+y, y, z'
'x, x-y, z'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-y+2/3, -x+1/3, z+1/3'
'-x+y+2/3, y+1/3, z+1/3'
'x+2/3, x-y+1/3, z+1/3'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'
'-y+1/3, -x+2/3, z+2/3'
'-x+y+1/3, y+2/3, z+2/3'
'x+1/3, x-y+2/3, z+2/3'

_cell_length_a                   16.4968(4)
_cell_length_b                   16.4968(4)
_cell_length_c                   13.5795(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     3200.47(17)
_cell_formula_units_Z            18
_cell_measurement_temperature    300(2)
_cell_measurement_reflns_used    9674
_cell_measurement_theta_min      3.22
_cell_measurement_theta_max      36.32

_exptl_crystal_description       block
_exptl_crystal_colour            green
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.893
_exptl_crystal_F_000             2570
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.050
_exptl_absorpt_coefficient_mu    7.845
_shelx_estimated_absorpt_T_min   0.508
_shelx_estimated_absorpt_T_max   0.695
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.2950
_exptl_absorpt_correction_T_max  0.3874
_exptl_absorpt_process_details   
;
 Reference: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D.,
 J. Appl. Cryst. 48 (2015) 3-10.
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      300(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker D8 QUEST'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            68364
_diffrn_reflns_av_unetI/netI     0.0059
_diffrn_reflns_av_R_equivalents  0.0278
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         3.222
_diffrn_reflns_theta_max         27.489
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measured_fraction_theta_full 0.985
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_Laue_measured_fraction_full 0.985
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_point_group_measured_fraction_full 0.985
_reflns_number_total             902
_reflns_number_gt                902
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2018/1 (Sheldrick, 2018)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0473P)²+56.5187P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   .
_refine_ls_hydrogen_treatment    undef
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         902
_refine_ls_number_parameters     43
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0327
_refine_ls_R_factor_gt           0.0327
_refine_ls_wR_factor_ref         0.0859
_refine_ls_wR_factor_gt          0.0859
_refine_ls_goodness_of_fit_ref   1.085
_refine_ls_restrained_S_all      1.085
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

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 0.000000 0.64492(2) 0.000000 0.01955(17) Uani 0.7 2 d S T P . .
Ca1 Ca 0.000000 0.64492(2) 0.000000 0.01955(17) Uani 0.3 2 d S T P . .
S1 S 0.19236(7) 0.80764(7) 0.00288(11) 0.0313(4) Uani 1 2 d S T P . .
S2 S -0.01938(8) 0.76347(9) -0.14869(8) 0.0277(3) Uani 1 1 d . . . . .
P1 P 0.15988(7) 0.84012(7) 0.13609(10) 0.0252(4) Uani 1 2 d S T P . .
S3 S 0.08787(12) 0.54394(6) 0.08992(12) 0.0273(3) Uani 1 2 d S T P . .
Cs1 Cs 0.333333 0.666667 0.166667 0.132(3) Uani 0.767(9) 12 d S T P . .
Cs2 Cs 0.000000 1.000000 0.000000 0.278(7) Uani 0.784(14) 12 d S T P . .
Cs3 Cs 0.000000 1.000000 -0.238(6) 0.48(7) Uani 0.125(7) 6 d S T P . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

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 S2 2.9376(12) . ?
Pr1 S2 2.9376(12) 6 ?
Pr1 S1 2.9596(3) 20_455 ?
Pr1 S1 2.9596(3) . ?
Pr1 S2 2.9625(11) 8_565 ?
Pr1 S2 2.9626(11) 16_454 ?
Pr1 S3 2.9636(10) 19_565 ?
Pr1 S3 2.9636(10) . ?
S1 P1 2.033(2) . ?
S2 P1 2.0259(16) 20_455 ?
S2 Cs3 3.94(3) . ?
P1 S3 2.055(2) 26_455 ?
S3 Cs1 3.6584(16) . ?
Cs1 Cs3 3.56(9) 13_545 ?
Cs1 Cs3 3.56(9) 31_564 ?
Cs2 Cs3 3.23(9) 19_575 ?
Cs2 Cs3 3.23(9) . ?

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
S2 Pr1 S2 87.86(5) . 6 ?
S2 Pr1 S1 68.67(4) . 20_455 ?
S2 Pr1 S1 80.18(4) 6 20_455 ?
S2 Pr1 S1 80.18(4) . . ?
S2 Pr1 S1 68.67(4) 6 . ?
S1 Pr1 S1 136.46(8) 20_455 . ?
S2 Pr1 S2 136.249(19) . 8_565 ?
S2 Pr1 S2 69.32(4) 6 8_565 ?
S1 Pr1 S2 70.90(4) 20_455 8_565 ?
S1 Pr1 S2 121.16(4) . 8_565 ?
S2 Pr1 S2 69.32(4) . 16_454 ?
S2 Pr1 S2 136.252(19) 6 16_454 ?
S1 Pr1 S2 121.16(4) 20_455 16_454 ?
S1 Pr1 S2 70.90(4) . 16_454 ?
S2 Pr1 S2 150.29(5) 8_565 16_454 ?
S2 Pr1 S3 104.94(4) . 19_565 ?
S2 Pr1 S3 154.70(4) 6 19_565 ?
S1 Pr1 S3 84.28(5) 20_455 19_565 ?
S1 Pr1 S3 134.27(5) . 19_565 ?
S2 Pr1 S3 86.80(4) 8_565 19_565 ?
S2 Pr1 S3 69.04(4) 16_454 19_565 ?
S2 Pr1 S3 154.70(4) . . ?
S2 Pr1 S3 104.94(3) 6 . ?
S1 Pr1 S3 134.27(5) 20_455 . ?
S1 Pr1 S3 84.28(5) . . ?
S2 Pr1 S3 69.04(4) 8_565 . ?
S2 Pr1 S3 86.80(4) 16_454 . ?
S3 Pr1 S3 72.45(5) 19_565 . ?
P1 S1 Pr1 86.93(3) . 21_665 ?
P1 S1 Pr1 86.93(3) . . ?
Pr1 S1 Pr1 163.47(8) 21_665 . ?
P1 S2 Pr1 87.66(5) 20_455 . ?
P1 S2 Pr1 90.23(6) 20_455 15_454 ?
Pr1 S2 Pr1 101.50(4) . 15_454 ?
P1 S2 Cs3 101.29(7) 20_455 . ?
Pr1 S2 Cs3 152.6(11) . . ?
Pr1 S2 Cs3 104.3(12) 15_454 . ?
S2 P1 S2 107.26(11) 21_665 6 ?
S2 P1 S1 110.07(6) 21_665 . ?
S2 P1 S1 110.07(6) 6 . ?
S2 P1 S3 110.73(6) 21_665 26_455 ?
S2 P1 S3 110.73(6) 6 26_455 ?
S1 P1 S3 108.00(11) . 26_455 ?
P1 S3 Pr1 89.62(5) 27 19_565 ?
P1 S3 Pr1 89.62(5) 27 . ?
Pr1 S3 Pr1 107.55(5) 19_565 . ?
P1 S3 Cs1 118.29(7) 27 . ?
Pr1 S3 Cs1 121.56(3) 19_565 . ?
Pr1 S3 Cs1 121.56(3) . . ?
Cs3 Cs1 Cs3 180.0 13_545 31_564 ?
Cs3 Cs1 S3 73.45(3) 13_545 25_565 ?
Cs3 Cs1 S3 106.55(3) 31_564 25_565 ?
Cs3 Cs1 S3 73.45(3) 13_545 27 ?
Cs3 Cs1 S3 106.55(3) 31_564 27 ?
S3 Cs1 S3 112.23(2) 25_565 27 ?
Cs3 Cs1 S3 106.55(3) 13_545 3_565 ?
Cs3 Cs1 S3 73.45(3) 31_564 3_565 ?
S3 Cs1 S3 67.77(2) 25_565 3_565 ?
S3 Cs1 S3 180.0 27 3_565 ?
Cs3 Cs1 S3 106.55(3) 13_545 . ?
Cs3 Cs1 S3 73.45(3) 31_564 . ?
S3 Cs1 S3 180.0 25_565 . ?
S3 Cs1 S3 67.77(2) 27 . ?
S3 Cs1 S3 112.23(2) 3_565 . ?
Cs3 Cs1 S3 106.55(3) 13_545 2_665 ?
Cs3 Cs1 S3 73.45(3) 31_564 2_665 ?
S3 Cs1 S3 67.77(2) 25_565 2_665 ?
S3 Cs1 S3 67.77(2) 27 2_665 ?
S3 Cs1 S3 112.23(2) 3_565 2_665 ?
S3 Cs1 S3 112.23(2) . 2_665 ?
Cs3 Cs1 S3 73.45(3) 13_545 26_455 ?
Cs3 Cs1 S3 106.55(3) 31_564 26_455 ?
S3 Cs1 S3 112.23(2) 25_565 26_455 ?
S3 Cs1 S3 112.23(2) 27 26_455 ?
S3 Cs1 S3 67.77(2) 3_565 26_455 ?
S3 Cs1 S3 67.77(2) . 26_455 ?
S3 Cs1 S3 180.0 2_665 26_455 ?
Cs3 Cs2 Cs3 180.0 19_575 . ?
Cs2 Cs3 Cs1 180.0 . 7_454 ?
Cs2 Cs3 S2 72.2(12) . 2_675 ?
Cs1 Cs3 S2 107.8(12) 7_454 2_675 ?
Cs2 Cs3 S2 72.2(12) . 22_665 ?
Cs1 Cs3 S2 107.8(12) 7_454 22_665 ?
S2 Cs3 S2 48.9(4) 2_675 22_665 ?
Cs2 Cs3 S2 72.2(12) . 23_455 ?
Cs1 Cs3 S2 107.8(12) 7_454 23_455 ?
S2 Cs3 S2 143(2) 2_675 23_455 ?
S2 Cs3 S2 111.1(11) 22_665 23_455 ?
Cs2 Cs3 S2 72.2(12) . 24_575 ?
Cs1 Cs3 S2 107.8(12) 7_454 24_575 ?
S2 Cs3 S2 64.8(5) 2_675 24_575 ?
S2 Cs3 S2 111.1(11) 22_665 24_575 ?
S2 Cs3 S2 111.1(11) 23_455 24_575 ?
Cs2 Cs3 S2 72.2(12) . 3_465 ?
Cs1 Cs3 S2 107.8(12) 7_454 3_465 ?
S2 Cs3 S2 111.1(11) 2_675 3_465 ?
S2 Cs3 S2 143(2) 22_665 3_465 ?
S2 Cs3 S2 64.8(5) 23_455 3_465 ?
S2 Cs3 S2 48.9(4) 24_575 3_465 ?
Cs2 Cs3 S2 72.2(12) . . ?
Cs1 Cs3 S2 107.8(12) 7_454 . ?
S2 Cs3 S2 111.1(11) 2_675 . ?
S2 Cs3 S2 64.8(5) 22_665 . ?
S2 Cs3 S2 48.9(4) 23_455 . ?
S2 Cs3 S2 143(2) 24_575 . ?
S2 Cs3 S2 111.1(11) 3_465 . ?

_refine_diff_density_max         3.370
_refine_diff_density_min         -4.618
_refine_diff_density_rms         0.203


# start Validation Reply Form
_vrf_PLAT974_1                   
;
PROBLEM: Check Calcd Negative Resid. Density on       Cs2      -4.72 eA-3  
RESPONSE: The cesium atoms are severely disordered along the channels in
the structure and cannot be located from the difference map. Due to this
they have been resolved as residing at three positions with overall 
occupancy equal to 0.15 to accomplish charge balance.
;
_vrf_PLAT214_1                   
;
PROBLEM: Atom Cs3       (Anion/Solvent) ADP max/min Ratio        5.8 prolat
RESPONSE: The cesium atoms are severely disordered along the channels in
the structure and cannot be located from the difference map. Due to this
they have been resolved as residing at three positions with overall 
occupancy equal to 0.15 to accomplish charge balance.
;
_vrf_PLAT971_1                   
;
PROBLEM: Check Calcd Resid. Dens.  0.86A   From Cs2             3.26 eA-3  
RESPONSE: The cesium atoms are severely disordered along the channels in
the structure and cannot be located from the difference map. Due to this
they have been resolved as residing at three positions with overall 
occupancy equal to 0.15 to accomplish charge balance.
;
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_Gd07
_database_code_depnum_ccdc_archive 'CCDC 2038462'
loop_
_audit_author_name
_audit_author_address
'Vladislav Klepov'
;University of South Carolina
United States of America
;
_audit_update_record             
;
2020-10-14 deposited with the CCDC.	2020-12-01 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/1
_shelx_SHELXL_version_number     2018/1
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'Ca0.30 Cs0.30 Gd0.70 P S4'
_chemical_formula_weight         321.18

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Ca Ca 0.2262 0.3064 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cs Cs -0.3680 2.1192 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Gd Gd -0.1653 3.9035 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 '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'

_space_group_crystal_system      trigonal
_space_group_IT_number           166
_space_group_name_H-M_alt        'R -3 m :H'
_space_group_name_Hall           '-R 3 2"'

_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.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'y, x, -z'
'x-y, -y, -z'
'-x, -x+y, -z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'y+2/3, x+1/3, -z+1/3'
'x-y+2/3, -y+1/3, -z+1/3'
'-x+2/3, -x+y+1/3, -z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'y+1/3, x+2/3, -z+2/3'
'x-y+1/3, -y+2/3, -z+2/3'
'-x+1/3, -x+y+2/3, -z+2/3'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-y, -x, z'
'-x+y, y, z'
'x, x-y, z'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-y+2/3, -x+1/3, z+1/3'
'-x+y+2/3, y+1/3, z+1/3'
'x+2/3, x-y+1/3, z+1/3'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'
'-y+1/3, -x+2/3, z+2/3'
'-x+y+1/3, y+2/3, z+2/3'
'x+1/3, x-y+2/3, z+2/3'

_cell_length_a                   16.3458(3)
_cell_length_b                   16.3458(3)
_cell_length_c                   13.4242(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     3106.21(13)
_cell_formula_units_Z            18
_cell_measurement_temperature    300(2)
_cell_measurement_reflns_used    9939
_cell_measurement_theta_min      3.25
_cell_measurement_theta_max      36.25

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    3.091
_exptl_crystal_F_000             2633
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.050
_exptl_absorpt_coefficient_mu    9.868
_shelx_estimated_absorpt_T_min   0.439
_shelx_estimated_absorpt_T_max   0.638
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.2278
_exptl_absorpt_correction_T_max  0.2740
_exptl_absorpt_process_details   
;
 Reference: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D.,
 J. Appl. Cryst. 48 (2015) 3-10.
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      300(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker D8 QUEST'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            62321
_diffrn_reflns_av_unetI/netI     0.0050
_diffrn_reflns_av_R_equivalents  0.0267
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         3.254
_diffrn_reflns_theta_max         27.491
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measured_fraction_theta_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_point_group_measured_fraction_full 0.989
_reflns_number_total             878
_reflns_number_gt                876
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2018/1 (Sheldrick, 2018)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0481P)²+63.0460P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   .
_refine_ls_hydrogen_treatment    undef
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         878
_refine_ls_number_parameters     43
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0323
_refine_ls_R_factor_gt           0.0323
_refine_ls_wR_factor_ref         0.0910
_refine_ls_wR_factor_gt          0.0910
_refine_ls_goodness_of_fit_ref   1.138
_refine_ls_restrained_S_all      1.137
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

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
Gd1 Gd 0.000000 0.64460(3) 0.000000 0.02114(18) Uani 0.7 2 d S T P . .
Ca1 Ca 0.000000 0.64460(3) 0.000000 0.02114(18) Uani 0.3 2 d S T P . .
S1 S 0.19337(8) 0.80663(8) 0.00200(12) 0.0316(4) Uani 1 2 d S T P . .
S2 S -0.01891(10) 0.76276(10) -0.14837(10) 0.0308(3) Uani 1 1 d . . . . .
P1 P 0.16071(8) 0.83929(8) 0.13635(12) 0.0269(4) Uani 1 2 d S T P . .
S3 S 0.08925(14) 0.54463(7) 0.08744(14) 0.0299(4) Uani 1 2 d S T P . .
Cs1 Cs 0.333333 0.666667 0.166667 0.151(4) Uani 0.739(11) 12 d S T P . .
Cs2 Cs 0.000000 1.000000 0.000000 0.238(6) Uani 0.723(13) 12 d S T P . .
Cs3 Cs 0.000000 1.000000 -0.264(5) 0.41(5) Uani 0.169(8) 6 d S T P . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

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
Gd1 S2 2.8965(14) 6 ?
Gd1 S2 2.8966(14) . ?
Gd1 S2 2.9249(14) 8_565 ?
Gd1 S2 2.9249(14) 16_454 ?
Gd1 S3 2.9258(11) . ?
Gd1 S3 2.9259(11) 19_565 ?
Gd1 S1 2.9385(4) . ?
Gd1 S1 2.9385(4) 20_455 ?
S1 P1 2.027(2) . ?
S1 Cs3 4.077(15) 31_564 ?
S2 P1 2.0254(19) 20_455 ?
S2 Cs3 4.04(2) . ?
P1 S3 2.053(3) 26_455 ?
S3 Cs1 3.615(2) . ?
S3 Cs3 4.05(3) 31_564 ?
Cs1 Cs3 3.17(6) 13_545 ?
Cs1 Cs3 3.17(6) 31_564 ?
Cs2 Cs3 3.54(6) 19_575 ?
Cs2 Cs3 3.54(6) . ?

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
S2 Gd1 S2 87.86(6) 6 . ?
S2 Gd1 S2 68.89(5) 6 8_565 ?
S2 Gd1 S2 136.17(2) . 8_565 ?
S2 Gd1 S2 136.17(2) 6 16_454 ?
S2 Gd1 S2 68.90(5) . 16_454 ?
S2 Gd1 S2 150.94(5) 8_565 16_454 ?
S2 Gd1 S3 105.43(4) 6 . ?
S2 Gd1 S3 153.84(5) . . ?
S2 Gd1 S3 69.98(5) 8_565 . ?
S2 Gd1 S3 86.39(5) 16_454 . ?
S2 Gd1 S3 153.84(5) 6 19_565 ?
S2 Gd1 S3 105.43(4) . 19_565 ?
S2 Gd1 S3 86.39(5) 8_565 19_565 ?
S2 Gd1 S3 69.97(5) 16_454 19_565 ?
S3 Gd1 S3 72.23(6) . 19_565 ?
S2 Gd1 S1 69.26(4) 6 . ?
S2 Gd1 S1 80.25(5) . . ?
S2 Gd1 S1 121.11(4) 8_565 . ?
S2 Gd1 S1 70.47(4) 16_454 . ?
S3 Gd1 S1 83.55(6) . . ?
S3 Gd1 S1 134.39(6) 19_565 . ?
S2 Gd1 S1 80.25(5) 6 20_455 ?
S2 Gd1 S1 69.26(4) . 20_455 ?
S2 Gd1 S1 70.47(4) 8_565 20_455 ?
S2 Gd1 S1 121.11(4) 16_454 20_455 ?
S3 Gd1 S1 134.39(6) . 20_455 ?
S3 Gd1 S1 83.55(6) 19_565 20_455 ?
S1 Gd1 S1 137.37(9) . 20_455 ?
P1 S1 Gd1 86.52(4) . 21_665 ?
P1 S1 Gd1 86.52(4) . . ?
Gd1 S1 Gd1 162.60(9) 21_665 . ?
P1 S1 Cs3 130.8(9) . 31_564 ?
Gd1 S1 Cs3 98.32(6) 21_665 31_564 ?
Gd1 S1 Cs3 98.31(6) . 31_564 ?
P1 S2 Gd1 87.68(6) 20_455 . ?
P1 S2 Gd1 89.76(7) 20_455 15_454 ?
Gd1 S2 Gd1 101.81(4) . 15_454 ?
P1 S2 Cs3 101.24(7) 20_455 . ?
Gd1 S2 Cs3 157.1(8) . . ?
Gd1 S2 Cs3 99.3(8) 15_454 . ?
S2 P1 S2 107.16(13) 21_665 6 ?
S2 P1 S1 109.84(8) 21_665 . ?
S2 P1 S1 109.84(8) 6 . ?
S2 P1 S3 110.70(7) 21_665 26_455 ?
S2 P1 S3 110.70(7) 6 26_455 ?
S1 P1 S3 108.61(13) . 26_455 ?
S2 P1 Ca1 55.46(5) 21_665 26_455 ?
S2 P1 Ca1 120.28(7) 6 26_455 ?
S1 P1 Ca1 129.87(6) . 26_455 ?
S3 P1 Ca1 55.48(4) 26_455 26_455 ?
S2 P1 Ca1 120.28(7) 21_665 8_565 ?
S2 P1 Ca1 55.46(5) 6 8_565 ?
S1 P1 Ca1 129.87(6) . 8_565 ?
S3 P1 Ca1 55.48(4) 26_455 8_565 ?
Ca1 P1 Ca1 83.47(4) 26_455 8_565 ?
P1 S3 Gd1 89.21(6) 27 . ?
P1 S3 Gd1 89.21(6) 27 19_565 ?
Gd1 S3 Gd1 107.77(6) . 19_565 ?
P1 S3 Cs1 117.13(9) 27 . ?
Gd1 S3 Cs1 122.06(4) . . ?
Gd1 S3 Cs1 122.05(4) 19_565 . ?
P1 S3 Cs3 165.6(8) 27 31_564 ?
Gd1 S3 Cs3 99.2(4) . 31_564 ?
Gd1 S3 Cs3 99.2(4) 19_565 31_564 ?
Cs1 S3 Cs3 48.5(7) . 31_564 ?
Cs3 Cs1 Cs3 180.0 13_545 31_564 ?
Cs3 Cs1 S3 72.89(3) 13_545 25_565 ?
Cs3 Cs1 S3 107.11(3) 31_564 25_565 ?
Cs3 Cs1 S3 72.89(3) 13_545 27 ?
Cs3 Cs1 S3 107.11(3) 31_564 27 ?
S3 Cs1 S3 111.73(3) 25_565 27 ?
Cs3 Cs1 S3 107.11(3) 13_545 3_565 ?
Cs3 Cs1 S3 72.89(3) 31_564 3_565 ?
S3 Cs1 S3 68.27(3) 25_565 3_565 ?
S3 Cs1 S3 180.0 27 3_565 ?
Cs3 Cs1 S3 107.11(3) 13_545 . ?
Cs3 Cs1 S3 72.89(3) 31_564 . ?
S3 Cs1 S3 180.0 25_565 . ?
S3 Cs1 S3 68.27(3) 27 . ?
S3 Cs1 S3 111.73(3) 3_565 . ?
Cs3 Cs1 S3 107.11(3) 13_545 2_665 ?
Cs3 Cs1 S3 72.89(3) 31_564 2_665 ?
S3 Cs1 S3 68.27(3) 25_565 2_665 ?
S3 Cs1 S3 68.27(3) 27 2_665 ?
S3 Cs1 S3 111.73(3) 3_565 2_665 ?
S3 Cs1 S3 111.73(3) . 2_665 ?
Cs3 Cs1 S3 72.89(3) 13_545 26_455 ?
Cs3 Cs1 S3 107.11(3) 31_564 26_455 ?
S3 Cs1 S3 111.73(3) 25_565 26_455 ?
S3 Cs1 S3 111.73(3) 27 26_455 ?
S3 Cs1 S3 68.27(3) 3_565 26_455 ?
S3 Cs1 S3 68.27(3) . 26_455 ?
S3 Cs1 S3 180.0 2_665 26_455 ?
Cs3 Cs2 Cs3 180.0 19_575 . ?
Cs1 Cs3 Cs2 180.0 7_454 . ?
Cs1 Cs3 S2 112.5(8) 7_454 . ?
Cs2 Cs3 S2 67.5(8) . . ?
Cs1 Cs3 S2 112.5(8) 7_454 2_675 ?
Cs2 Cs3 S2 67.5(8) . 2_675 ?
S2 Cs3 S2 106.2(9) . 2_675 ?
Cs1 Cs3 S2 112.5(8) 7_454 22_665 ?
Cs2 Cs3 S2 67.5(8) . 22_665 ?
S2 Cs3 S2 62.4(4) . 22_665 ?
S2 Cs3 S2 47.6(3) 2_675 22_665 ?
Cs1 Cs3 S2 112.5(8) 7_454 24_575 ?
Cs2 Cs3 S2 67.5(8) . 24_575 ?
S2 Cs3 S2 134.2(16) . 24_575 ?
S2 Cs3 S2 62.4(4) 2_675 24_575 ?
S2 Cs3 S2 106.2(9) 22_665 24_575 ?
Cs1 Cs3 S2 112.5(8) 7_454 23_455 ?
Cs2 Cs3 S2 67.5(8) . 23_455 ?
S2 Cs3 S2 47.6(3) . 23_455 ?
S2 Cs3 S2 134.2(16) 2_675 23_455 ?
S2 Cs3 S2 106.2(9) 22_665 23_455 ?
S2 Cs3 S2 106.2(9) 24_575 23_455 ?
Cs1 Cs3 S2 112.5(8) 7_454 3_465 ?
Cs2 Cs3 S2 67.5(8) . 3_465 ?
S2 Cs3 S2 106.2(9) . 3_465 ?
S2 Cs3 S2 106.2(9) 2_675 3_465 ?
S2 Cs3 S2 134.2(16) 22_665 3_465 ?
S2 Cs3 S2 47.6(3) 24_575 3_465 ?
S2 Cs3 S2 62.4(4) 23_455 3_465 ?
Cs1 Cs3 S3 58.6(7) 7_454 32_454 ?
Cs2 Cs3 S3 121.4(7) . 32_454 ?
S2 Cs3 S3 148.5(4) . 32_454 ?
S2 Cs3 S3 104.84(16) 2_675 32_454 ?
S2 Cs3 S3 148.5(4) 22_665 32_454 ?
S2 Cs3 S3 59.35(8) 24_575 32_454 ?
S2 Cs3 S3 104.84(16) 23_455 32_454 ?
S2 Cs3 S3 59.35(8) 3_465 32_454 ?
Cs1 Cs3 S3 58.6(7) 7_454 33_554 ?
Cs2 Cs3 S3 121.4(7) . 33_554 ?
S2 Cs3 S3 59.35(8) . 33_554 ?
S2 Cs3 S3 148.5(4) 2_675 33_554 ?
S2 Cs3 S3 104.84(16) 22_665 33_554 ?
S2 Cs3 S3 148.5(4) 24_575 33_554 ?
S2 Cs3 S3 59.35(8) 23_455 33_554 ?
S2 Cs3 S3 104.84(16) 3_465 33_554 ?
S3 Cs3 S3 95.3(10) 32_454 33_554 ?
Cs1 Cs3 S3 58.6(7) 7_454 31_564 ?
Cs2 Cs3 S3 121.4(7) . 31_564 ?
S2 Cs3 S3 104.84(16) . 31_564 ?
S2 Cs3 S3 59.35(8) 2_675 31_564 ?
S2 Cs3 S3 59.35(8) 22_665 31_564 ?
S2 Cs3 S3 104.84(16) 24_575 31_564 ?
S2 Cs3 S3 148.5(4) 23_455 31_564 ?
S2 Cs3 S3 148.5(4) 3_465 31_564 ?
S3 Cs3 S3 95.3(10) 32_454 31_564 ?
S3 Cs3 S3 95.3(10) 33_554 31_564 ?
Cs1 Cs3 S1 76.4(8) 7_454 33_554 ?
Cs2 Cs3 S1 103.6(8) . 33_554 ?
S2 Cs3 S1 91.49(13) . 33_554 ?
S2 Cs3 S1 153.9(6) 2_675 33_554 ?
S2 Cs3 S1 153.9(6) 22_665 33_554 ?
S2 Cs3 S1 91.49(13) 24_575 33_554 ?
S2 Cs3 S1 49.24(6) 23_455 33_554 ?
S2 Cs3 S1 49.24(6) 3_465 33_554 ?
S3 Cs3 S1 57.5(4) 32_454 33_554 ?
S3 Cs3 S1 57.5(4) 33_554 33_554 ?
S3 Cs3 S1 135.0(16) 31_564 33_554 ?

_refine_diff_density_max         3.695
_refine_diff_density_min         -3.794
_refine_diff_density_rms         0.216



# start Validation Reply Form
_vrf_PLAT971_1                   
;
PROBLEM: Check Calcd Resid. Dens.  1.05A   From Cs2             3.69 eA-3  
RESPONSE: The cesium atoms are severely disordered along the channels in
the structure and cannot be located from the difference map. Due to this
they have been resolved as residing at three positions with overall 
occupancy equal to 0.15 to accomplish charge balance.
;
_vrf_PLAT974_1                   
;
PROBLEM: Check Calcd Negative Resid. Density on       Cs2      -3.88 eA-3  
RESPONSE: The cesium atoms are severely disordered along the channels in
the structure and cannot be located from the difference map. Due to this
they have been resolved as residing at three positions with overall 
occupancy equal to 0.15 to accomplish charge balance.
;
_vrf_PLAT214_1                   
;
PROBLEM: Atom Cs3       (Anion/Solvent) ADP max/min Ratio        5.6 prolat
RESPONSE: The cesium atoms are severely disordered along the channels in
the structure and cannot be located from the difference map. Due to this
they have been resolved as residing at three positions with overall 
occupancy equal to 0.15 to accomplish charge balance.
;
_vrf_PLAT260_1                   
;
PROBLEM: Large Average Ueq of Residue Including       Cs3      0.405 Check 
RESPONSE: The cesium atoms are severely disordered along the channels in
the structure and cannot be located from the difference map. Due to this
they have been resolved as residing at three positions with overall 
occupancy equal to 0.15 to accomplish charge balance.
;
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_Gd05
_database_code_depnum_ccdc_archive 'CCDC 2038468'
loop_
_audit_author_name
_audit_author_address
'Vladislav Klepov'
;University of South Carolina
United States of America
;
_audit_update_record             
;
2020-10-14 deposited with the CCDC.	2020-12-01 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/1
_shelx_SHELXL_version_number     2018/1
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'Ca0.50 Cs0.50 Gd0.50 P S4'
_chemical_formula_weight         324.33

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
P P 0.1023 0.0942 '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'
Ca Ca 0.2262 0.3064 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cs Cs -0.3680 2.1192 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Gd Gd -0.1653 3.9035 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 2/c'
_space_group_name_Hall           '-C 2yc'

_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.
;

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'

_cell_length_a                   9.1603(2)
_cell_length_b                   9.1898(2)
_cell_length_c                   16.6882(4)
_cell_angle_alpha                90
_cell_angle_beta                 103.6865(8)
_cell_angle_gamma                90
_cell_volume                     1364.94(5)
_cell_formula_units_Z            8
_cell_measurement_temperature    300(2)
_cell_measurement_reflns_used    9161
_cell_measurement_theta_min      3.19
_cell_measurement_theta_max      36.28

_exptl_crystal_description       plate
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    3.157
_exptl_crystal_F_000             1188
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.060
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.010
_exptl_absorpt_coefficient_mu    9.274
_shelx_estimated_absorpt_T_min   0.606
_shelx_estimated_absorpt_T_max   0.913
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.1717
_exptl_absorpt_correction_T_max  0.2740
_exptl_absorpt_process_details   
;
 Reference: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D.,
 J. Appl. Cryst. 48 (2015) 3-10.
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      300(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker D8 QUEST'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            35177
_diffrn_reflns_av_unetI/netI     0.0105
_diffrn_reflns_av_R_equivalents  0.0287
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         3.186
_diffrn_reflns_theta_max         29.988
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measured_fraction_theta_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_point_group_measured_fraction_full 0.990
_reflns_number_total             1975
_reflns_number_gt                1956
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2018/1 (Sheldrick, 2018)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0080P)²+7.6916P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   .
_refine_ls_hydrogen_treatment    undef
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         1975
_refine_ls_number_parameters     60
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0192
_refine_ls_R_factor_gt           0.0190
_refine_ls_wR_factor_ref         0.0404
_refine_ls_wR_factor_gt          0.0403
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_restrained_S_all      1.039
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

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
Cs1 Cs 0.000000 0.64396(3) 0.250000 0.03184(6) Uani 1 2 d S T P . .
Gd1 Gd 0.49358(2) 0.73189(2) 0.02434(2) 0.02577(6) Uani 0.5 1 d . . P . .
Ca1 Ca 0.49358(2) 0.73189(2) 0.02434(2) 0.02577(6) Uani 0.5 1 d . . P . .
P1 P 0.27431(6) 0.48505(6) 0.09110(4) 0.01854(11) Uani 1 1 d . . . . .
S1 S 0.25185(7) 0.70200(6) 0.11029(4) 0.02645(12) Uani 1 1 d . . . . .
S2 S 0.18070(7) 0.36029(7) 0.16485(4) 0.02444(11) Uani 1 1 d . . . . .
S3 S 0.50029(7) 0.45451(7) 0.11067(4) 0.02700(12) Uani 1 1 d . . . . .
S4 S 0.17846(10) 0.44064(10) -0.03038(4) 0.0449(2) Uani 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

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
Cs1 S2 3.5439(6) 4 ?
Cs1 S2 3.5439(6) 3_455 ?
Cs1 S2 3.5592(6) . ?
Cs1 S2 3.5592(6) 2 ?
Cs1 S3 3.6816(7) 4 ?
Cs1 S3 3.6816(7) 3_455 ?
Cs1 S1 3.6862(6) . ?
Cs1 S1 3.6863(6) 2 ?
Cs1 S4 3.7248(7) 5_565 ?
Cs1 S4 3.7248(7) 6_566 ?
Cs1 Gd1 4.7320(2) 8_466 ?
Cs1 Gd1 4.7320(2) 7_565 ?
Ca1 S2 2.8154(7) 3 ?
Ca1 S3 2.8415(7) 5_665 ?
Ca1 S1 2.8426(7) 7_565 ?
Ca1 S4 2.8485(7) 3 ?
Ca1 S3 2.9215(7) . ?
Ca1 S1 2.9222(7) . ?
Ca1 S4 3.3773(11) 5_665 ?
Ca1 P1 3.3883(6) . ?
Ca1 S4 3.4095(11) 7_565 ?
Ca1 P1 3.4511(6) 3 ?
P1 S2 2.0159(8) . ?
P1 S3 2.0373(8) . ?
P1 S1 2.0374(8) . ?
P1 S4 2.0506(9) . ?

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
S2 Cs1 S2 111.75(2) 4 3_455 ?
S2 Cs1 S2 98.817(7) 4 . ?
S2 Cs1 S2 131.947(18) 3_455 . ?
S2 Cs1 S2 131.947(18) 4 2 ?
S2 Cs1 S2 98.817(7) 3_455 2 ?
S2 Cs1 S2 85.821(19) . 2 ?
S2 Cs1 S3 55.651(13) 4 4 ?
S2 Cs1 S3 72.213(15) 3_455 4 ?
S2 Cs1 S3 152.850(14) . 4 ?
S2 Cs1 S3 104.224(13) 2 4 ?
S2 Cs1 S3 72.213(15) 4 3_455 ?
S2 Cs1 S3 55.651(13) 3_455 3_455 ?
S2 Cs1 S3 104.224(13) . 3_455 ?
S2 Cs1 S3 152.850(14) 2 3_455 ?
S3 Cs1 S3 78.36(2) 4 3_455 ?
S2 Cs1 S1 65.908(14) 4 . ?
S2 Cs1 S1 104.233(14) 3_455 . ?
S2 Cs1 S1 55.504(13) . . ?
S2 Cs1 S1 141.104(14) 2 . ?
S3 Cs1 S1 112.419(14) 4 . ?
S3 Cs1 S1 52.720(13) 3_455 . ?
S2 Cs1 S1 104.233(14) 4 2 ?
S2 Cs1 S1 65.909(14) 3_455 2 ?
S2 Cs1 S1 141.104(14) . 2 ?
S2 Cs1 S1 55.505(13) 2 2 ?
S3 Cs1 S1 52.721(13) 4 2 ?
S3 Cs1 S1 112.420(14) 3_455 2 ?
S1 Cs1 S1 163.36(2) . 2 ?
S2 Cs1 S4 129.796(15) 4 5_565 ?
S2 Cs1 S4 66.054(19) 3_455 5_565 ?
S2 Cs1 S4 65.893(19) . 5_565 ?
S2 Cs1 S4 95.893(15) 2 5_565 ?
S3 Cs1 S4 135.85(2) 4 5_565 ?
S3 Cs1 S4 66.803(16) 3_455 5_565 ?
S1 Cs1 S4 66.577(16) . 5_565 ?
S1 Cs1 S4 117.253(17) 2 5_565 ?
S2 Cs1 S4 66.054(19) 4 6_566 ?
S2 Cs1 S4 129.796(14) 3_455 6_566 ?
S2 Cs1 S4 95.893(15) . 6_566 ?
S2 Cs1 S4 65.894(19) 2 6_566 ?
S3 Cs1 S4 66.803(16) 4 6_566 ?
S3 Cs1 S4 135.85(2) 3_455 6_566 ?
S1 Cs1 S4 117.253(17) . 6_566 ?
S1 Cs1 S4 66.577(16) 2 6_566 ?
S4 Cs1 S4 155.90(3) 5_565 6_566 ?
S2 Cs1 Gd1 71.024(10) 4 8_466 ?
S2 Cs1 Gd1 93.135(10) 3_455 8_466 ?
S2 Cs1 Gd1 132.553(10) . 8_466 ?
S2 Cs1 Gd1 71.150(10) 2 8_466 ?
S3 Cs1 Gd1 36.875(11) 4 8_466 ?
S3 Cs1 Gd1 115.224(12) 3_455 8_466 ?
S1 Cs1 Gd1 136.883(11) . 8_466 ?
S1 Cs1 Gd1 36.896(10) 2 8_466 ?
S4 Cs1 Gd1 154.062(14) 5_565 8_466 ?
S4 Cs1 Gd1 37.002(11) 6_566 8_466 ?
S2 Cs1 Gd1 93.135(10) 4 7_565 ?
S2 Cs1 Gd1 71.024(10) 3_455 7_565 ?
S2 Cs1 Gd1 71.149(10) . 7_565 ?
S2 Cs1 Gd1 132.552(10) 2 7_565 ?
S3 Cs1 Gd1 115.224(12) 4 7_565 ?
S3 Cs1 Gd1 36.875(11) 3_455 7_565 ?
S1 Cs1 Gd1 36.896(10) . 7_565 ?
S1 Cs1 Gd1 136.883(11) 2 7_565 ?
S4 Cs1 Gd1 37.002(11) 5_565 7_565 ?
S4 Cs1 Gd1 154.062(15) 6_566 7_565 ?
Gd1 Cs1 Gd1 152.098(8) 8_466 7_565 ?
S2 Ca1 S3 142.251(19) 3 5_665 ?
S2 Ca1 S1 141.303(19) 3 7_565 ?
S3 Ca1 S1 70.275(18) 5_665 7_565 ?
S2 Ca1 S4 72.167(18) 3 3 ?
S3 Ca1 S4 91.55(2) 5_665 3 ?
S1 Ca1 S4 91.25(2) 7_565 3 ?
S2 Ca1 S3 90.993(19) 3 . ?
S3 Ca1 S3 82.12(2) 5_665 . ?
S1 Ca1 S3 119.777(19) 7_565 . ?
S4 Ca1 S3 143.22(2) 3 . ?
S2 Ca1 S1 90.764(18) 3 . ?
S3 Ca1 S1 119.469(19) 5_665 . ?
S1 Ca1 S1 81.87(2) 7_565 . ?
S4 Ca1 S1 142.91(2) 3 . ?
S3 Ca1 S1 66.788(17) . . ?
S2 Ca1 S4 79.043(18) 3 5_665 ?
S3 Ca1 S4 63.660(17) 5_665 5_665 ?
S1 Ca1 S4 130.959(18) 7_565 5_665 ?
S4 Ca1 S4 74.55(3) 3 5_665 ?
S3 Ca1 S4 70.177(17) . 5_665 ?
S1 Ca1 S4 135.498(18) . 5_665 ?
S2 Ca1 P1 107.350(16) 3 . ?
S3 Ca1 P1 88.944(17) 5_665 . ?
S1 Ca1 P1 89.050(17) 7_565 . ?
S4 Ca1 P1 179.489(19) 3 . ?
S3 Ca1 P1 36.740(15) . . ?
S1 Ca1 P1 36.741(15) . . ?
S4 Ca1 P1 105.558(17) 5_665 . ?
S2 Ca1 S4 78.466(18) 3 7_565 ?
S3 Ca1 S4 130.658(18) 5_665 7_565 ?
S1 Ca1 S4 63.261(17) 7_565 7_565 ?
S4 Ca1 S4 74.28(3) 3 7_565 ?
S3 Ca1 S4 135.353(18) . 7_565 ?
S1 Ca1 S4 70.076(17) . 7_565 ?
S4 Ca1 S4 145.85(2) 5_665 7_565 ?
P1 Ca1 S4 105.490(16) . 7_565 ?
S2 Ca1 P1 35.740(15) 3 3 ?
S3 Ca1 P1 120.620(16) 5_665 3 ?
S1 Ca1 P1 120.041(17) 7_565 3 ?
S4 Ca1 P1 36.427(17) 3 3 ?
S3 Ca1 P1 120.123(17) . 3 ?
S1 Ca1 P1 119.883(17) . 3 ?
S4 Ca1 P1 73.575(16) 5_665 3 ?
P1 Ca1 P1 143.090(19) . 3 ?
S4 Ca1 P1 73.130(16) 7_565 3 ?
S2 Ca1 Cs1 124.073(13) 3 7_565 ?
S3 Ca1 Cs1 51.031(14) 5_665 7_565 ?
S1 Ca1 Cs1 51.126(13) 7_565 7_565 ?
S4 Ca1 Cs1 51.906(14) 3 7_565 ?
S3 Ca1 Cs1 133.145(14) . 7_565 ?
S1 Ca1 Cs1 132.990(14) . 7_565 ?
S4 Ca1 Cs1 85.841(12) 5_665 7_565 ?
P1 Ca1 Cs1 128.576(11) . 7_565 ?
S4 Ca1 Cs1 85.839(12) 7_565 7_565 ?
P1 Ca1 Cs1 88.333(10) 3 7_565 ?
S2 P1 S3 112.74(4) . . ?
S2 P1 S1 112.78(4) . . ?
S3 P1 S1 104.25(4) . . ?
S2 P1 S4 110.24(4) . . ?
S3 P1 S4 108.19(4) . . ?
S1 P1 S4 108.34(4) . . ?
S2 P1 Ca1 162.25(3) . . ?
S3 P1 Ca1 59.07(2) . . ?
S1 P1 Ca1 59.09(2) . . ?
S4 P1 Ca1 87.52(3) . . ?
P1 S1 Gd1 100.10(3) . 7_565 ?
P1 S1 Ca1 84.17(3) . . ?
Gd1 S1 Ca1 98.13(2) 7_565 . ?
P1 S1 Cs1 93.41(3) . . ?
Gd1 S1 Cs1 91.978(17) 7_565 . ?
Ca1 S1 Cs1 169.87(2) . . ?
P1 S2 Gd1 89.60(3) . 3_445 ?
P1 S2 Cs1 97.70(3) . 3_545 ?
Gd1 S2 Cs1 112.390(19) 3_445 3_545 ?
P1 S2 Cs1 97.61(3) . . ?
Gd1 S2 Cs1 112.984(19) 3_445 . ?
Cs1 S2 Cs1 131.947(18) 3_545 . ?
P1 S3 Gd1 99.55(3) . 5_665 ?
P1 S3 Ca1 84.19(3) . . ?
Gd1 S3 Ca1 97.88(2) 5_665 . ?
P1 S3 Cs1 93.18(3) . 3_545 ?
Gd1 S3 Cs1 92.094(18) 5_665 3_545 ?
Ca1 S3 Cs1 169.98(2) . 3_545 ?
P1 S4 Gd1 88.00(3) . 3_445 ?
P1 S4 Cs1 179.09(3) . 5_565 ?
Gd1 S4 Cs1 91.092(19) 3_445 5_565 ?

_refine_diff_density_max         0.927
_refine_diff_density_min         -1.113
_refine_diff_density_rms         0.095

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_Nd05
_database_code_depnum_ccdc_archive 'CCDC 2038466'
loop_
_audit_author_name
_audit_author_address
'Vladislav Klepov'
;University of South Carolina
United States of America
;
_audit_update_record             
;
2020-10-14 deposited with the CCDC.	2020-12-01 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/1
_shelx_SHELXL_version_number     2018/1
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'Ca0.50 Cs0.50 Nd0.50 P S4'
_chemical_formula_weight         317.83

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Cs Cs -0.3680 2.1192 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Nd Nd -0.1943 3.0179 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 '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'
Ca Ca 0.2262 0.3064 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 2/c'
_space_group_name_Hall           '-C 2yc'

_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.
;

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'

_cell_length_a                   9.1970(2)
_cell_length_b                   9.2233(2)
_cell_length_c                   16.7149(4)
_cell_angle_alpha                90
_cell_angle_beta                 103.8709(8)
_cell_angle_gamma                90
_cell_volume                     1376.52(5)
_cell_formula_units_Z            8
_cell_measurement_temperature    300(2)
_cell_measurement_reflns_used    9894
_cell_measurement_theta_min      3.18
_cell_measurement_theta_max      34.57

_exptl_crystal_description       plate
_exptl_crystal_colour            blue
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    3.067
_exptl_crystal_F_000             1172
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.02
_exptl_absorpt_coefficient_mu    8.150
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.3999
_exptl_absorpt_correction_T_max  0.4969
_exptl_absorpt_process_details   
;
 Reference: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D.,
 J. Appl. Cryst. 48 (2015) 3-10.
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      300(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker D8 QUEST'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            17462
_diffrn_reflns_av_unetI/netI     0.0215
_diffrn_reflns_av_R_equivalents  0.0545
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         2.510
_diffrn_reflns_theta_max         28.492
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measured_fraction_theta_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_point_group_measured_fraction_full 0.993
_reflns_number_total             1748
_reflns_number_gt                1678
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2018/1 (Sheldrick, 2018)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0370P)²+4.0316P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   .
_refine_ls_hydrogen_treatment    undef
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         1748
_refine_ls_number_parameters     60
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0259
_refine_ls_R_factor_gt           0.0250
_refine_ls_wR_factor_ref         0.0668
_refine_ls_wR_factor_gt          0.0661
_refine_ls_goodness_of_fit_ref   1.109
_refine_ls_restrained_S_all      1.109
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

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
Cs1 Cs 0.000000 0.64272(3) 0.250000 0.03319(10) Uani 1 2 d S T P . .
Nd1 Nd 0.49349(3) 0.73180(3) 0.02455(2) 0.02460(9) Uani 0.5 1 d . . P . .
Ca1 Ca 0.49349(3) 0.73180(3) 0.02455(2) 0.02460(9) Uani 0.5 1 d . . P . .
P1 P 0.27602(8) 0.48556(7) 0.09253(4) 0.01933(15) Uani 1 1 d . . . . .
S1 S 0.25309(9) 0.70155(8) 0.11238(5) 0.02608(16) Uani 1 1 d . . . . .
S2 S 0.18271(9) 0.36086(8) 0.16578(5) 0.02436(16) Uani 1 1 d . . . . .
S3 S 0.50115(8) 0.45427(8) 0.11271(5) 0.02668(16) Uani 1 1 d . . . . .
S4 S 0.18108(12) 0.44345(12) -0.02943(5) 0.0436(2) Uani 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

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
Cs1 S2 3.5461(8) 4 ?
Cs1 S2 3.5461(8) 3_455 ?
Cs1 S2 3.5635(8) . ?
Cs1 S2 3.5635(8) 2 ?
Cs1 S3 3.6790(8) 4 ?
Cs1 S3 3.6790(8) 3_455 ?
Cs1 S1 3.6840(8) . ?
Cs1 S1 3.6840(8) 2 ?
Cs1 S4 3.7489(8) 5_565 ?
Cs1 S4 3.7489(8) 6_566 ?
Cs1 Nd1 4.7469(3) 8_466 ?
Cs1 Nd1 4.7469(3) 7_565 ?
Ca1 S2 2.8370(8) 3 ?
Ca1 S3 2.8749(8) 5_665 ?
Ca1 S1 2.8758(8) 7_565 ?
Ca1 S4 2.8891(9) 3 ?
Ca1 S1 2.9458(8) . ?
Ca1 S3 2.9460(8) . ?
Ca1 S4 3.3853(13) 5_665 ?
Ca1 P1 3.3970(7) . ?
Ca1 S4 3.4086(13) 7_565 ?
Ca1 P1 3.4793(7) 3 ?
P1 S2 2.0154(10) . ?
P1 S3 2.0370(10) . ?
P1 S1 2.0387(10) . ?
P1 S4 2.0532(11) . ?

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
S2 Cs1 S2 110.87(3) 4 3_455 ?
S2 Cs1 S2 98.606(9) 4 . ?
S2 Cs1 S2 132.70(2) 3_455 . ?
S2 Cs1 S2 132.70(2) 4 2 ?
S2 Cs1 S2 98.606(9) 3_455 2 ?
S2 Cs1 S2 86.30(2) . 2 ?
S2 Cs1 S3 55.555(17) 4 4 ?
S2 Cs1 S3 71.297(18) 3_455 4 ?
S2 Cs1 S3 152.671(17) . 4 ?
S2 Cs1 S3 104.552(16) 2 4 ?
S2 Cs1 S3 71.297(18) 4 3_455 ?
S2 Cs1 S3 55.555(17) 3_455 3_455 ?
S2 Cs1 S3 104.552(16) . 3_455 ?
S2 Cs1 S3 152.671(17) 2 3_455 ?
S3 Cs1 S3 77.29(3) 4 3_455 ?
S2 Cs1 S1 65.250(17) 4 . ?
S2 Cs1 S1 104.569(17) 3_455 . ?
S2 Cs1 S1 55.416(15) . . ?
S2 Cs1 S1 141.491(18) 2 . ?
S3 Cs1 S1 111.790(17) 4 . ?
S3 Cs1 S1 53.039(16) 3_455 . ?
S2 Cs1 S1 104.568(17) 4 2 ?
S2 Cs1 S1 65.250(17) 3_455 2 ?
S2 Cs1 S1 141.492(18) . 2 ?
S2 Cs1 S1 55.416(15) 2 2 ?
S3 Cs1 S1 53.039(16) 4 2 ?
S3 Cs1 S1 111.789(17) 3_455 2 ?
S1 Cs1 S1 163.06(2) . 2 ?
S2 Cs1 S4 129.789(18) 4 5_565 ?
S2 Cs1 S4 66.46(2) 3_455 5_565 ?
S2 Cs1 S4 66.25(2) . 5_565 ?
S2 Cs1 S4 95.363(18) 2 5_565 ?
S3 Cs1 S4 135.40(2) 4 5_565 ?
S3 Cs1 S4 67.615(19) 3_455 5_565 ?
S1 Cs1 S4 67.38(2) . 5_565 ?
S1 Cs1 S4 116.56(2) 2 5_565 ?
S2 Cs1 S4 66.46(2) 4 6_566 ?
S2 Cs1 S4 129.789(18) 3_455 6_566 ?
S2 Cs1 S4 95.363(18) . 6_566 ?
S2 Cs1 S4 66.25(2) 2 6_566 ?
S3 Cs1 S4 67.615(19) 4 6_566 ?
S3 Cs1 S4 135.40(2) 3_455 6_566 ?
S1 Cs1 S4 116.56(2) . 6_566 ?
S1 Cs1 S4 67.38(2) 2 6_566 ?
S4 Cs1 S4 155.52(3) 5_565 6_566 ?
S2 Cs1 Nd1 71.204(12) 4 8_466 ?
S2 Cs1 Nd1 92.612(13) 3_455 8_466 ?
S2 Cs1 Nd1 132.547(13) . 8_466 ?
S2 Cs1 Nd1 71.309(12) 2 8_466 ?
S3 Cs1 Nd1 37.249(13) 4 8_466 ?
S3 Cs1 Nd1 114.531(14) 3_455 8_466 ?
S1 Cs1 Nd1 136.389(13) . 8_466 ?
S1 Cs1 Nd1 37.264(13) 2 8_466 ?
S4 Cs1 Nd1 153.745(18) 5_565 8_466 ?
S4 Cs1 Nd1 37.490(13) 6_566 8_466 ?
S2 Cs1 Nd1 92.612(13) 4 7_565 ?
S2 Cs1 Nd1 71.204(12) 3_455 7_565 ?
S2 Cs1 Nd1 71.308(12) . 7_565 ?
S2 Cs1 Nd1 132.547(13) 2 7_565 ?
S3 Cs1 Nd1 114.531(14) 4 7_565 ?
S3 Cs1 Nd1 37.249(13) 3_455 7_565 ?
S1 Cs1 Nd1 37.265(13) . 7_565 ?
S1 Cs1 Nd1 136.389(13) 2 7_565 ?
S4 Cs1 Nd1 37.490(13) 5_565 7_565 ?
S4 Cs1 Nd1 153.745(18) 6_566 7_565 ?
Nd1 Cs1 Nd1 151.779(9) 8_466 7_565 ?
S2 Ca1 S3 142.19(2) 3 5_665 ?
S2 Ca1 S1 141.44(2) 3 7_565 ?
S3 Ca1 S1 69.74(2) 5_665 7_565 ?
S2 Ca1 S4 71.53(2) 3 3 ?
S3 Ca1 S4 91.63(3) 5_665 3 ?
S1 Ca1 S4 91.32(3) 7_565 3 ?
S2 Ca1 S1 90.52(2) 3 . ?
S3 Ca1 S1 119.98(2) 5_665 . ?
S1 Ca1 S1 82.76(2) 7_565 . ?
S4 Ca1 S1 142.69(3) 3 . ?
S2 Ca1 S3 90.69(2) 3 . ?
S3 Ca1 S3 82.97(2) 5_665 . ?
S1 Ca1 S3 120.23(2) 7_565 . ?
S4 Ca1 S3 143.02(3) 3 . ?
S1 Ca1 S3 66.37(2) . . ?
S2 Ca1 S4 79.51(2) 3 5_665 ?
S3 Ca1 S4 63.26(2) 5_665 5_665 ?
S1 Ca1 S4 130.18(2) 7_565 5_665 ?
S4 Ca1 S4 74.90(3) 3 5_665 ?
S1 Ca1 S4 135.04(2) . 5_665 ?
S3 Ca1 S4 70.01(2) . 5_665 ?
S2 Ca1 P1 107.16(2) 3 . ?
S3 Ca1 P1 89.54(2) 5_665 . ?
S1 Ca1 P1 89.65(2) 7_565 . ?
S4 Ca1 P1 178.68(2) 3 . ?
S1 Ca1 P1 36.631(18) . . ?
S3 Ca1 P1 36.597(19) . . ?
S4 Ca1 P1 105.12(2) 5_665 . ?
S2 Ca1 S4 79.04(2) 3 7_565 ?
S3 Ca1 S4 129.94(2) 5_665 7_565 ?
S1 Ca1 S4 62.94(2) 7_565 7_565 ?
S4 Ca1 S4 74.56(3) 3 7_565 ?
S1 Ca1 S4 69.95(2) . 7_565 ?
S3 Ca1 S4 134.95(2) . 7_565 ?
S4 Ca1 S4 146.91(3) 5_665 7_565 ?
P1 Ca1 S4 105.13(2) . 7_565 ?
S2 Ca1 P1 35.400(19) 3 3 ?
S3 Ca1 P1 120.52(2) 5_665 3 ?
S1 Ca1 P1 120.06(2) 7_565 3 ?
S4 Ca1 P1 36.13(2) 3 3 ?
S1 Ca1 P1 119.47(2) . 3 ?
S3 Ca1 P1 119.65(2) . 3 ?
S4 Ca1 P1 74.13(2) 5_665 3 ?
P1 Ca1 P1 142.56(2) . 3 ?
S4 Ca1 P1 73.75(2) 7_565 3 ?
S2 Ca1 Cs1 123.694(16) 3 7_565 ?
S3 Ca1 Cs1 50.764(16) 5_665 7_565 ?
S1 Ca1 Cs1 50.865(16) 7_565 7_565 ?
S4 Ca1 Cs1 52.161(17) 3 7_565 ?
S1 Ca1 Cs1 133.613(17) . 7_565 ?
S3 Ca1 Cs1 133.715(17) . 7_565 ?
S4 Ca1 Cs1 85.626(15) 5_665 7_565 ?
P1 Ca1 Cs1 129.144(14) . 7_565 ?
S4 Ca1 Cs1 85.646(15) 7_565 7_565 ?
P1 Ca1 Cs1 88.294(13) 3 7_565 ?
S2 P1 S3 112.49(5) . . ?
S2 P1 S1 112.53(4) . . ?
S3 P1 S1 104.61(4) . . ?
S2 P1 S4 110.70(5) . . ?
S3 P1 S4 108.12(5) . . ?
S1 P1 S4 108.09(5) . . ?
S2 P1 Ca1 162.81(4) . . ?
S3 P1 Ca1 59.57(3) . . ?
S1 P1 Ca1 59.56(3) . . ?
S4 P1 Ca1 86.49(3) . . ?
P1 S1 Nd1 99.90(4) . 7_565 ?
P1 S1 Ca1 83.81(3) . . ?
Nd1 S1 Ca1 97.24(2) 7_565 . ?
P1 S1 Cs1 93.62(3) . . ?
Nd1 S1 Cs1 91.87(2) 7_565 . ?
Ca1 S1 Cs1 170.83(3) . . ?
P1 S2 Nd1 89.97(3) . 3_445 ?
P1 S2 Cs1 97.77(3) . 3_545 ?
Nd1 S2 Cs1 112.00(2) 3_445 3_545 ?
P1 S2 Cs1 97.67(3) . . ?
Nd1 S2 Cs1 112.43(2) 3_445 . ?
Cs1 S2 Cs1 132.70(2) 3_545 . ?
P1 S3 Nd1 99.42(4) . 5_665 ?
P1 S3 Ca1 83.84(3) . . ?
Nd1 S3 Ca1 97.03(2) 5_665 . ?
P1 S3 Cs1 93.39(3) . 3_545 ?
Nd1 S3 Cs1 91.99(2) 5_665 3_545 ?
Ca1 S3 Cs1 170.88(3) . 3_545 ?
P1 S4 Nd1 87.79(3) . 3_445 ?
P1 S4 Cs1 178.14(4) . 5_565 ?
Nd1 S4 Cs1 90.35(2) 3_445 5_565 ?

_refine_diff_density_max         1.480
_refine_diff_density_min         -0.946
_refine_diff_density_rms         0.151

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_Dy05
_database_code_depnum_ccdc_archive 'CCDC 2038470'
loop_
_audit_author_name
_audit_author_address
'Vladislav Klepov'
;University of South Carolina
United States of America
;
_audit_update_record             
;
2020-10-14 deposited with the CCDC.	2020-12-01 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/1
_shelx_SHELXL_version_number     2018/1
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'Ca0.50 Cs0.50 Dy0.50 P S4'
_chemical_formula_weight         326.96

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
P P 0.1023 0.0942 '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'
Ca Ca 0.2262 0.3064 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cs Cs -0.3680 2.1192 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Dy Dy -0.1892 4.4098 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 2/c'
_space_group_name_Hall           '-C 2yc'

_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.
;

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'

_cell_length_a                   9.1378(2)
_cell_length_b                   9.1727(2)
_cell_length_c                   16.6704(4)
_cell_angle_alpha                90
_cell_angle_beta                 103.6778(8)
_cell_angle_gamma                90
_cell_volume                     1357.66(5)
_cell_formula_units_Z            8
_cell_measurement_temperature    300(2)
_cell_measurement_reflns_used    9694
_cell_measurement_theta_min      3.19
_cell_measurement_theta_max      36.33

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    3.199
_exptl_crystal_F_000             1196
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.240
_exptl_crystal_size_mid          0.060
_exptl_crystal_size_min          0.060
_exptl_absorpt_coefficient_mu    9.942
_shelx_estimated_absorpt_T_min   0.199
_shelx_estimated_absorpt_T_max   0.587
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.1560
_exptl_absorpt_correction_T_max  0.2740
_exptl_absorpt_process_details   
;
 Reference: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D.,
 J. Appl. Cryst. 48 (2015) 3-10.
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      300(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker D8 QUEST'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            49642
_diffrn_reflns_av_unetI/netI     0.0134
_diffrn_reflns_av_R_equivalents  0.0417
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         3.193
_diffrn_reflns_theta_max         29.999
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measured_fraction_theta_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_point_group_measured_fraction_full 0.994
_reflns_number_total             1972
_reflns_number_gt                1963
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2018/1 (Sheldrick, 2018)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0152P)²+9.9262P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   .
_refine_ls_hydrogen_treatment    undef
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         1972
_refine_ls_number_parameters     60
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0238
_refine_ls_R_factor_gt           0.0237
_refine_ls_wR_factor_ref         0.0522
_refine_ls_wR_factor_gt          0.0521
_refine_ls_goodness_of_fit_ref   1.086
_refine_ls_restrained_S_all      1.086
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

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
Cs1 Cs 0.000000 0.64404(3) 0.250000 0.03151(8) Uani 1 2 d S T P . .
Dy1 Dy 0.49359(3) 0.73177(3) 0.02417(2) 0.02689(7) Uani 0.5 1 d . . P . .
Ca1 Ca 0.49359(3) 0.73177(3) 0.02417(2) 0.02689(7) Uani 0.5 1 d . . P . .
P1 P 0.27353(8) 0.48469(8) 0.09036(4) 0.01802(13) Uani 1 1 d . . . . .
S1 S 0.25141(9) 0.70220(8) 0.10928(5) 0.02713(15) Uani 1 1 d . . . . .
S2 S 0.17977(9) 0.35969(8) 0.16425(5) 0.02499(14) Uani 1 1 d . . . . .
S3 S 0.50009(8) 0.45453(9) 0.10964(5) 0.02775(15) Uani 1 1 d . . . . .
S4 S 0.17684(13) 0.43921(13) -0.03093(5) 0.0455(3) Uani 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

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
Cs1 S2 3.5413(8) 4 ?
Cs1 S2 3.5413(8) 3_455 ?
Cs1 S2 3.5575(8) 2 ?
Cs1 S2 3.5575(8) . ?
Cs1 S3 3.6860(8) 4 ?
Cs1 S3 3.6860(8) 3_455 ?
Cs1 S1 3.6897(8) . ?
Cs1 S1 3.6897(8) 2 ?
Cs1 S4 3.7067(8) 5_565 ?
Cs1 S4 3.7067(8) 6_566 ?
Cs1 Dy1 4.7241(3) 8_466 ?
Cs1 Dy1 4.7241(3) 7_565 ?
Ca1 S2 2.8010(8) 3 ?
Ca1 S3 2.8214(9) 5_665 ?
Ca1 S1 2.8236(8) 7_565 ?
Ca1 S4 2.8277(9) 3 ?
Ca1 S3 2.9088(9) . ?
Ca1 S1 2.9102(8) . ?
Ca1 S4 3.3736(13) 5_665 ?
Ca1 P1 3.3834(7) . ?
Ca1 S4 3.4102(14) 7_565 ?
Ca1 P1 3.4363(7) 3 ?
P1 S2 2.0161(10) . ?
P1 S1 2.0374(10) . ?
P1 S3 2.0375(10) . ?
P1 S4 2.0490(11) . ?

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
S2 Cs1 S2 112.08(3) 4 3_455 ?
S2 Cs1 S2 131.55(2) 4 2 ?
S2 Cs1 S2 98.961(9) 3_455 2 ?
S2 Cs1 S2 98.961(9) 4 . ?
S2 Cs1 S2 131.55(2) 3_455 . ?
S2 Cs1 S2 85.69(2) 2 . ?
S2 Cs1 S3 55.692(16) 4 4 ?
S2 Cs1 S3 72.570(18) 3_455 4 ?
S2 Cs1 S3 104.002(16) 2 4 ?
S2 Cs1 S3 153.000(17) . 4 ?
S2 Cs1 S3 72.570(19) 4 3_455 ?
S2 Cs1 S3 55.692(16) 3_455 3_455 ?
S2 Cs1 S3 153.000(17) 2 3_455 ?
S2 Cs1 S3 104.002(16) . 3_455 ?
S3 Cs1 S3 78.82(3) 4 3_455 ?
S2 Cs1 S1 66.210(17) 4 . ?
S2 Cs1 S1 103.997(17) 3_455 . ?
S2 Cs1 S1 141.039(18) 2 . ?
S2 Cs1 S1 55.557(16) . . ?
S3 Cs1 S1 112.676(18) 4 . ?
S3 Cs1 S1 52.489(16) 3_455 . ?
S2 Cs1 S1 103.997(17) 4 2 ?
S2 Cs1 S1 66.210(17) 3_455 2 ?
S2 Cs1 S1 55.557(16) 2 2 ?
S2 Cs1 S1 141.038(18) . 2 ?
S3 Cs1 S1 52.489(16) 4 2 ?
S3 Cs1 S1 112.676(18) 3_455 2 ?
S1 Cs1 S1 163.38(2) . 2 ?
S2 Cs1 S4 129.710(18) 4 5_565 ?
S2 Cs1 S4 65.87(2) 3_455 5_565 ?
S2 Cs1 S4 96.298(19) 2 5_565 ?
S2 Cs1 S4 65.68(2) . 5_565 ?
S3 Cs1 S4 135.98(3) 4 5_565 ?
S3 Cs1 S4 66.38(2) 3_455 5_565 ?
S1 Cs1 S4 66.13(2) . 5_565 ?
S1 Cs1 S4 117.66(2) 2 5_565 ?
S2 Cs1 S4 65.87(2) 4 6_566 ?
S2 Cs1 S4 129.710(18) 3_455 6_566 ?
S2 Cs1 S4 65.68(2) 2 6_566 ?
S2 Cs1 S4 96.298(19) . 6_566 ?
S3 Cs1 S4 66.38(2) 4 6_566 ?
S3 Cs1 S4 135.98(3) 3_455 6_566 ?
S1 Cs1 S4 117.66(2) . 6_566 ?
S1 Cs1 S4 66.13(2) 2 6_566 ?
S4 Cs1 S4 156.22(4) 5_565 6_566 ?
S2 Cs1 Dy1 70.904(12) 4 8_466 ?
S2 Cs1 Dy1 93.312(13) 3_455 8_466 ?
S2 Cs1 Dy1 71.062(12) 2 8_466 ?
S2 Cs1 Dy1 132.696(13) . 8_466 ?
S3 Cs1 Dy1 36.643(13) 4 8_466 ?
S3 Cs1 Dy1 115.452(15) 3_455 8_466 ?
S1 Cs1 Dy1 137.077(14) . 8_466 ?
S1 Cs1 Dy1 36.680(13) 2 8_466 ?
S4 Cs1 Dy1 154.237(18) 5_565 8_466 ?
S4 Cs1 Dy1 36.751(14) 6_566 8_466 ?
S2 Cs1 Dy1 93.312(13) 4 7_565 ?
S2 Cs1 Dy1 70.904(12) 3_455 7_565 ?
S2 Cs1 Dy1 132.696(13) 2 7_565 ?
S2 Cs1 Dy1 71.063(12) . 7_565 ?
S3 Cs1 Dy1 115.452(15) 4 7_565 ?
S3 Cs1 Dy1 36.643(13) 3_455 7_565 ?
S1 Cs1 Dy1 36.679(13) . 7_565 ?
S1 Cs1 Dy1 137.077(14) 2 7_565 ?
S4 Cs1 Dy1 36.751(13) 5_565 7_565 ?
S4 Cs1 Dy1 154.237(18) 6_566 7_565 ?
Dy1 Cs1 Dy1 152.094(10) 8_466 7_565 ?
S2 Ca1 S3 142.27(2) 3 5_665 ?
S2 Ca1 S1 141.18(2) 3 7_565 ?
S3 Ca1 S1 70.59(2) 5_665 7_565 ?
S2 Ca1 S4 72.50(2) 3 3 ?
S3 Ca1 S4 91.51(3) 5_665 3 ?
S1 Ca1 S4 91.14(3) 7_565 3 ?
S2 Ca1 S3 91.14(2) 3 . ?
S3 Ca1 S3 81.72(2) 5_665 . ?
S1 Ca1 S3 119.61(2) 7_565 . ?
S4 Ca1 S3 143.36(3) 3 . ?
S2 Ca1 S1 90.83(2) 3 . ?
S3 Ca1 S1 119.28(2) 5_665 . ?
S1 Ca1 S1 81.46(2) 7_565 . ?
S4 Ca1 S1 142.95(3) 3 . ?
S3 Ca1 S1 67.01(2) . . ?
S2 Ca1 S4 78.78(2) 3 5_665 ?
S3 Ca1 S4 63.89(2) 5_665 5_665 ?
S1 Ca1 S4 131.40(2) 7_565 5_665 ?
S4 Ca1 S4 74.41(4) 3 5_665 ?
S3 Ca1 S4 70.28(2) . 5_665 ?
S1 Ca1 S4 135.73(2) . 5_665 ?
S2 Ca1 P1 107.42(2) 3 . ?
S3 Ca1 P1 88.68(2) 5_665 . ?
S1 Ca1 P1 88.80(2) 7_565 . ?
S4 Ca1 P1 179.76(3) 3 . ?
S3 Ca1 P1 36.819(18) . . ?
S1 Ca1 P1 36.815(19) . . ?
S4 Ca1 P1 105.81(2) 5_665 . ?
S2 Ca1 S4 78.10(2) 3 7_565 ?
S3 Ca1 S4 131.08(2) 5_665 7_565 ?
S1 Ca1 S4 63.45(2) 7_565 7_565 ?
S4 Ca1 S4 74.06(4) 3 7_565 ?
S3 Ca1 S4 135.57(2) . 7_565 ?
S1 Ca1 S4 70.15(2) . 7_565 ?
S4 Ca1 S4 145.22(3) 5_665 7_565 ?
P1 Ca1 S4 105.71(2) . 7_565 ?
S2 Ca1 P1 35.923(18) 3 3 ?
S3 Ca1 P1 120.66(2) 5_665 3 ?
S1 Ca1 P1 119.97(2) 7_565 3 ?
S4 Ca1 P1 36.58(2) 3 3 ?
S3 Ca1 P1 120.37(2) . 3 ?
S1 Ca1 P1 120.04(2) . 3 ?
S4 Ca1 P1 73.28(2) 5_665 3 ?
P1 Ca1 P1 143.34(2) . 3 ?
S4 Ca1 P1 72.72(2) 7_565 3 ?
S2 Ca1 Cs1 124.162(16) 3 7_565 ?
S3 Ca1 Cs1 51.236(17) 5_665 7_565 ?
S1 Ca1 Cs1 51.312(17) 7_565 7_565 ?
S4 Ca1 Cs1 51.660(17) 3 7_565 ?
S3 Ca1 Cs1 132.943(18) . 7_565 ?
S1 Ca1 Cs1 132.767(17) . 7_565 ?
S4 Ca1 Cs1 85.945(15) 5_665 7_565 ?
P1 Ca1 Cs1 128.415(14) . 7_565 ?
S4 Ca1 Cs1 85.920(15) 7_565 7_565 ?
P1 Ca1 Cs1 88.239(12) 3 7_565 ?
S2 P1 S1 112.97(4) . . ?
S2 P1 S3 112.90(5) . . ?
S1 P1 S3 104.05(5) . . ?
S2 P1 S4 109.92(5) . . ?
S1 P1 S4 108.47(5) . . ?
S3 P1 S4 108.24(5) . . ?
S2 P1 Ca1 162.06(4) . . ?
S1 P1 Ca1 58.86(3) . . ?
S3 P1 Ca1 58.82(3) . . ?
S4 P1 Ca1 88.02(3) . . ?
P1 S1 Dy1 100.21(4) . 7_565 ?
P1 S1 Ca1 84.32(3) . . ?
Dy1 S1 Ca1 98.54(2) 7_565 . ?
P1 S1 Cs1 93.23(3) . . ?
Dy1 S1 Cs1 92.01(2) 7_565 . ?
Ca1 S1 Cs1 169.43(3) . . ?
P1 S2 Dy1 89.48(3) . 3_445 ?
P1 S2 Cs1 97.72(3) . 3_545 ?
Dy1 S2 Cs1 112.55(2) 3_445 3_545 ?
P1 S2 Cs1 97.58(3) . . ?
Dy1 S2 Cs1 113.27(2) 3_445 . ?
Cs1 S2 Cs1 131.55(2) 3_545 . ?
P1 S3 Dy1 99.64(4) . 5_665 ?
P1 S3 Ca1 84.36(3) . . ?
Dy1 S3 Ca1 98.29(2) 5_665 . ?
P1 S3 Cs1 93.00(3) . 3_545 ?
Dy1 S3 Cs1 92.12(2) 5_665 3_545 ?
Ca1 S3 Cs1 169.55(3) . 3_545 ?
P1 S4 Dy1 88.09(3) . 3_445 ?
P1 S4 Cs1 179.66(4) . 5_565 ?
Dy1 S4 Cs1 91.59(2) 3_445 5_565 ?

_refine_diff_density_max         0.836
_refine_diff_density_min         -1.440
_refine_diff_density_rms         0.137

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_Tb05
_database_code_depnum_ccdc_archive 'CCDC 2038469'
loop_
_audit_author_name
_audit_author_address
'Vladislav Klepov'
;University of South Carolina
United States of America
;
_audit_update_record             
;
2020-10-14 deposited with the CCDC.	2020-12-01 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/1
_shelx_SHELXL_version_number     2018/1
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'Ca0.50 Cs0.50 P S4 Tb0.50'
_chemical_formula_weight         325.17

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
P P 0.1023 0.0942 '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'
Ca Ca 0.2262 0.3064 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cs Cs -0.3680 2.1192 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Tb Tb -0.1723 4.1537 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 2/c'
_space_group_name_Hall           '-C 2yc'

_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.
;

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'

_cell_length_a                   9.1479(4)
_cell_length_b                   9.1800(4)
_cell_length_c                   16.6874(7)
_cell_angle_alpha                90
_cell_angle_beta                 103.6882(15)
_cell_angle_gamma                90
_cell_volume                     1361.57(10)
_cell_formula_units_Z            8
_cell_measurement_temperature    300(2)
_cell_measurement_reflns_used    9915
_cell_measurement_theta_min      3.19
_cell_measurement_theta_max      36.28

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    3.173
_exptl_crystal_F_000             1192
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.080
_exptl_crystal_size_mid          0.060
_exptl_crystal_size_min          0.030
_exptl_absorpt_coefficient_mu    9.620
_shelx_estimated_absorpt_T_min   0.513
_shelx_estimated_absorpt_T_max   0.761
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.1768
_exptl_absorpt_correction_T_max  0.2740
_exptl_absorpt_process_details   
;
 Reference: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D.,
 J. Appl. Cryst. 48 (2015) 3-10.
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      300(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker D8 QUEST'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            25062
_diffrn_reflns_av_unetI/netI     0.0141
_diffrn_reflns_av_R_equivalents  0.0356
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         2.512
_diffrn_reflns_theta_max         27.490
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measured_fraction_theta_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_point_group_measured_fraction_full 0.995
_reflns_number_total             1562
_reflns_number_gt                1551
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2018/1 (Sheldrick, 2018)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0014P)²+34.6131P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   .
_refine_ls_hydrogen_treatment    undef
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         1562
_refine_ls_number_parameters     60
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0313
_refine_ls_R_factor_gt           0.0311
_refine_ls_wR_factor_ref         0.0744
_refine_ls_wR_factor_gt          0.0743
_refine_ls_goodness_of_fit_ref   1.140
_refine_ls_restrained_S_all      1.140
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

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
Cs1 Cs 0.000000 0.64405(6) 0.250000 0.03261(15) Uani 1 2 d S T P . .
Tb1 Tb 0.49354(5) 0.73176(5) 0.02426(3) 0.02756(14) Uani 0.5 1 d . . P . .
Ca1 Ca 0.49354(5) 0.73176(5) 0.02426(3) 0.02756(14) Uani 0.5 1 d . . P . .
P1 P 0.27373(16) 0.48483(15) 0.09069(9) 0.0196(3) Uani 1 1 d . . . . .
S1 S 0.25160(18) 0.70197(16) 0.10975(10) 0.0277(3) Uani 1 1 d . . . . .
S2 S 0.18023(17) 0.35991(16) 0.16454(9) 0.0259(3) Uani 1 1 d . . . . .
S3 S 0.50004(16) 0.45446(17) 0.11006(10) 0.0283(3) Uani 1 1 d . . . . .
S4 S 0.1775(2) 0.4398(2) -0.03066(10) 0.0462(5) Uani 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

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
Cs1 S2 3.5417(16) 4 ?
Cs1 S2 3.5417(16) 3_455 ?
Cs1 S2 3.5592(16) 2 ?
Cs1 S2 3.5592(16) . ?
Cs1 S3 3.6843(16) 4 ?
Cs1 S3 3.6843(16) 3_455 ?
Cs1 S1 3.6888(16) 2 ?
Cs1 S1 3.6888(16) . ?
Cs1 S4 3.7167(17) 5_565 ?
Cs1 S4 3.7167(17) 6_566 ?
Cs1 Tb1 4.7306(5) 8_466 ?
Cs1 Tb1 4.7306(5) 7_565 ?
Ca1 S2 2.8086(16) 3 ?
Ca1 S3 2.8306(17) 5_665 ?
Ca1 S1 2.8331(16) 7_565 ?
Ca1 S4 2.8371(17) 3 ?
Ca1 S3 2.9143(16) . ?
Ca1 S1 2.9159(16) . ?
Ca1 S4 3.375(3) 5_665 ?
Ca1 P1 3.3861(15) . ?
Ca1 S4 3.411(3) 7_565 ?
Ca1 P1 3.4425(15) 3 ?
P1 S2 2.016(2) . ?
P1 S1 2.036(2) . ?
P1 S3 2.038(2) . ?
P1 S4 2.050(2) . ?

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
S2 Cs1 S2 111.95(5) 4 3_455 ?
S2 Cs1 S2 131.72(4) 4 2 ?
S2 Cs1 S2 98.895(17) 3_455 2 ?
S2 Cs1 S2 98.895(17) 4 . ?
S2 Cs1 S2 131.72(4) 3_455 . ?
S2 Cs1 S2 85.75(5) 2 . ?
S2 Cs1 S3 55.66(3) 4 4 ?
S2 Cs1 S3 72.45(4) 3_455 4 ?
S2 Cs1 S3 104.08(3) 2 4 ?
S2 Cs1 S3 152.91(3) . 4 ?
S2 Cs1 S3 72.45(4) 4 3_455 ?
S2 Cs1 S3 55.66(3) 3_455 3_455 ?
S2 Cs1 S3 152.91(3) 2 3_455 ?
S2 Cs1 S3 104.08(3) . 3_455 ?
S3 Cs1 S3 78.67(5) 4 3_455 ?
S2 Cs1 S1 104.11(3) 4 2 ?
S2 Cs1 S1 66.10(3) 3_455 2 ?
S2 Cs1 S1 55.51(3) 2 2 ?
S2 Cs1 S1 141.04(4) . 2 ?
S3 Cs1 S1 52.61(3) 4 2 ?
S3 Cs1 S1 112.60(3) 3_455 2 ?
S2 Cs1 S1 66.10(3) 4 . ?
S2 Cs1 S1 104.11(3) 3_455 . ?
S2 Cs1 S1 141.04(4) 2 . ?
S2 Cs1 S1 55.51(3) . . ?
S3 Cs1 S1 112.60(4) 4 . ?
S3 Cs1 S1 52.60(3) 3_455 . ?
S1 Cs1 S1 163.42(5) 2 . ?
S2 Cs1 S4 129.73(4) 4 5_565 ?
S2 Cs1 S4 65.95(5) 3_455 5_565 ?
S2 Cs1 S4 96.14(4) 2 5_565 ?
S2 Cs1 S4 65.77(5) . 5_565 ?
S3 Cs1 S4 135.95(5) 4 5_565 ?
S3 Cs1 S4 66.51(4) 3_455 5_565 ?
S1 Cs1 S4 117.51(4) 2 5_565 ?
S1 Cs1 S4 66.29(4) . 5_565 ?
S2 Cs1 S4 65.95(5) 4 6_566 ?
S2 Cs1 S4 129.73(4) 3_455 6_566 ?
S2 Cs1 S4 65.77(5) 2 6_566 ?
S2 Cs1 S4 96.14(4) . 6_566 ?
S3 Cs1 S4 66.51(4) 4 6_566 ?
S3 Cs1 S4 135.95(5) 3_455 6_566 ?
S1 Cs1 S4 66.29(4) 2 6_566 ?
S1 Cs1 S4 117.51(4) . 6_566 ?
S4 Cs1 S4 156.10(7) 5_565 6_566 ?
S2 Cs1 Tb1 70.96(2) 4 8_466 ?
S2 Cs1 Tb1 93.24(3) 3_455 8_466 ?
S2 Cs1 Tb1 71.09(2) 2 8_466 ?
S2 Cs1 Tb1 132.63(3) . 8_466 ?
S3 Cs1 Tb1 36.72(3) 4 8_466 ?
S3 Cs1 Tb1 115.39(3) 3_455 8_466 ?
S1 Cs1 Tb1 36.76(3) 2 8_466 ?
S1 Cs1 Tb1 137.02(3) . 8_466 ?
S4 Cs1 Tb1 154.17(3) 5_565 8_466 ?
S4 Cs1 Tb1 36.84(3) 6_566 8_466 ?
S2 Cs1 Tb1 93.24(3) 4 7_565 ?
S2 Cs1 Tb1 70.96(2) 3_455 7_565 ?
S2 Cs1 Tb1 132.63(3) 2 7_565 ?
S2 Cs1 Tb1 71.09(2) . 7_565 ?
S3 Cs1 Tb1 115.39(3) 4 7_565 ?
S3 Cs1 Tb1 36.72(3) 3_455 7_565 ?
S1 Cs1 Tb1 137.02(3) 2 7_565 ?
S1 Cs1 Tb1 36.76(3) . 7_565 ?
S4 Cs1 Tb1 36.84(3) 5_565 7_565 ?
S4 Cs1 Tb1 154.17(3) 6_566 7_565 ?
Tb1 Cs1 Tb1 152.108(19) 8_466 7_565 ?
S2 Ca1 S3 142.23(5) 3 5_665 ?
S2 Ca1 S1 141.22(5) 3 7_565 ?
S3 Ca1 S1 70.46(4) 5_665 7_565 ?
S2 Ca1 S4 72.37(5) 3 3 ?
S3 Ca1 S4 91.47(5) 5_665 3 ?
S1 Ca1 S4 91.13(5) 7_565 3 ?
S2 Ca1 S3 91.07(5) 3 . ?
S3 Ca1 S3 81.93(5) 5_665 . ?
S1 Ca1 S3 119.71(5) 7_565 . ?
S4 Ca1 S3 143.31(6) 3 . ?
S2 Ca1 S1 90.79(4) 3 . ?
S3 Ca1 S1 119.41(5) 5_665 . ?
S1 Ca1 S1 81.70(5) 7_565 . ?
S4 Ca1 S1 142.96(6) 3 . ?
S3 Ca1 S1 66.88(4) . . ?
S2 Ca1 S4 78.89(4) 3 5_665 ?
S3 Ca1 S4 63.76(4) 5_665 5_665 ?
S1 Ca1 S4 131.17(4) 7_565 5_665 ?
S4 Ca1 S4 74.43(7) 3 5_665 ?
S3 Ca1 S4 70.28(4) . 5_665 ?
S1 Ca1 S4 135.64(4) . 5_665 ?
S2 Ca1 P1 107.38(4) 3 . ?
S3 Ca1 P1 88.86(4) 5_665 . ?
S1 Ca1 P1 88.95(4) 7_565 . ?
S4 Ca1 P1 179.67(5) 3 . ?
S3 Ca1 P1 36.78(4) . . ?
S1 Ca1 P1 36.75(4) . . ?
S4 Ca1 P1 105.74(4) 5_665 . ?
S2 Ca1 S4 78.26(4) 3 7_565 ?
S3 Ca1 S4 130.87(4) 5_665 7_565 ?
S1 Ca1 S4 63.35(4) 7_565 7_565 ?
S4 Ca1 S4 74.14(7) 3 7_565 ?
S3 Ca1 S4 135.49(4) . 7_565 ?
S1 Ca1 S4 70.16(4) . 7_565 ?
S4 Ca1 S4 145.46(6) 5_665 7_565 ?
P1 Ca1 S4 105.62(4) . 7_565 ?
S2 Ca1 P1 35.84(4) 3 3 ?
S3 Ca1 P1 120.61(4) 5_665 3 ?
S1 Ca1 P1 119.95(4) 7_565 3 ?
S4 Ca1 P1 36.52(4) 3 3 ?
S3 Ca1 P1 120.28(4) . 3 ?
S1 Ca1 P1 119.95(4) . 3 ?
S4 Ca1 P1 73.41(4) 5_665 3 ?
P1 Ca1 P1 143.22(5) . 3 ?
S4 Ca1 P1 72.87(4) 7_565 3 ?
S2 Ca1 Cs1 124.13(3) 3 7_565 ?
S3 Ca1 Cs1 51.10(3) 5_665 7_565 ?
S1 Ca1 Cs1 51.19(3) 7_565 7_565 ?
S4 Ca1 Cs1 51.76(3) 3 7_565 ?
S3 Ca1 Cs1 133.03(4) . 7_565 ?
S1 Ca1 Cs1 132.89(3) . 7_565 ?
S4 Ca1 Cs1 85.86(3) 5_665 7_565 ?
P1 Ca1 Cs1 128.49(3) . 7_565 ?
S4 Ca1 Cs1 85.87(3) 7_565 7_565 ?
P1 Ca1 Cs1 88.29(3) 3 7_565 ?
S2 P1 S1 112.90(9) . . ?
S2 P1 S3 112.79(9) . . ?
S1 P1 S3 104.12(9) . . ?
S2 P1 S4 110.12(9) . . ?
S1 P1 S4 108.45(10) . . ?
S3 P1 S4 108.16(10) . . ?
S2 P1 Ca1 162.11(8) . . ?
S1 P1 Ca1 58.97(6) . . ?
S3 P1 Ca1 58.92(6) . . ?
S4 P1 Ca1 87.77(6) . . ?
P1 S1 Tb1 100.15(7) . 7_565 ?
P1 S1 Ca1 84.28(6) . . ?
Tb1 S1 Ca1 98.30(5) 7_565 . ?
P1 S1 Cs1 93.33(6) . . ?
Tb1 S1 Cs1 92.04(4) 7_565 . ?
Ca1 S1 Cs1 169.64(6) . . ?
P1 S2 Tb1 89.49(7) . 3_445 ?
P1 S2 Cs1 97.75(7) . 3_545 ?
Tb1 S2 Cs1 112.50(5) 3_445 3_545 ?
P1 S2 Cs1 97.58(7) . . ?
Tb1 S2 Cs1 113.14(5) 3_445 . ?
Cs1 S2 Cs1 131.72(4) 3_545 . ?
P1 S3 Tb1 99.66(7) . 5_665 ?
P1 S3 Ca1 84.30(6) . . ?
Tb1 S3 Ca1 98.07(5) 5_665 . ?
P1 S3 Cs1 93.09(6) . 3_545 ?
Tb1 S3 Cs1 92.17(4) 5_665 3_545 ?
Ca1 S3 Cs1 169.71(6) . 3_545 ?
P1 S4 Tb1 88.02(7) . 3_445 ?
P1 S4 Cs1 179.41(9) . 5_565 ?
Tb1 S4 Cs1 91.40(5) 3_445 5_565 ?

_refine_diff_density_max         1.045
_refine_diff_density_min         -0.964
_refine_diff_density_rms         0.165

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_Dy07
_database_code_depnum_ccdc_archive 'CCDC 2038464'
loop_
_audit_author_name
_audit_author_address
'Vladislav Klepov'
;University of South Carolina
United States of America
;
_audit_update_record             
;
2020-10-14 deposited with the CCDC.	2020-12-01 downloaded from the CCDC.
;
_audit_creation_date             2019-07-03
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         '0.06(Ca5.4 Cs5.4 Dy12.6 P18 S72)'
_chemical_formula_sum            'Ca0.30 Cs0.30 Dy0.70 P S4'
_chemical_formula_weight         324.86
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Ca Ca 0.2262 0.3064 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cs Cs -0.3680 2.1192 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Dy Dy -0.1892 4.4098 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 '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'

_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.
;
_space_group_crystal_system      trigonal
_space_group_IT_number           166
_space_group_name_H-M_alt        'R -3 m'
_space_group_name_Hall           '-R 3 2"'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'y, x, -z'
'x-y, -y, -z'
'-x, -x+y, -z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'y+2/3, x+1/3, -z+1/3'
'x-y+2/3, -y+1/3, -z+1/3'
'-x+2/3, -x+y+1/3, -z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'y+1/3, x+2/3, -z+2/3'
'x-y+1/3, -y+2/3, -z+2/3'
'-x+1/3, -x+y+2/3, -z+2/3'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-y, -x, z'
'-x+y, y, z'
'x, x-y, z'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-y+2/3, -x+1/3, z+1/3'
'-x+y+2/3, y+1/3, z+1/3'
'x+2/3, x-y+1/3, z+1/3'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'
'-y+1/3, -x+2/3, z+2/3'
'-x+y+1/3, y+2/3, z+2/3'
'x+1/3, x-y+2/3, z+2/3'

_cell_length_a                   16.3288(4)
_cell_length_b                   16.3288(4)
_cell_length_c                   13.3220(4)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     3076.16(18)
_cell_formula_units_Z            18
_cell_measurement_reflns_used    9871
_cell_measurement_temperature    301(2)
_cell_measurement_theta_max      32.93
_cell_measurement_theta_min      2.49
_shelx_estimated_absorpt_T_max   0.899
_shelx_estimated_absorpt_T_min   0.813
_exptl_absorpt_coefficient_mu    10.825
_exptl_absorpt_correction_T_max  0.2694
_exptl_absorpt_correction_T_min  0.2252
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0649 before and 0.0582 after correction.
The Ratio of minimum to maximum transmission is 0.8359.
The λ/2 correction factor is Not present.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    3.156
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       shard
_exptl_crystal_F_000             2659
_exptl_crystal_size_max          0.02
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.01
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0355
_diffrn_reflns_av_unetI/netI     0.0101
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            23058
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.496
_diffrn_reflns_theta_min         2.495
_diffrn_ambient_temperature      301.39
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker D8 QUEST'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                830
_reflns_number_total             878
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       ?
_computing_data_collection       ?
_computing_data_reduction        ?
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    ?
_refine_diff_density_max         3.721
_refine_diff_density_min         -3.719
_refine_diff_density_rms         0.217
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.140
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     43
_refine_ls_number_reflns         878
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0327
_refine_ls_R_factor_gt           0.0311
_refine_ls_restrained_S_all      1.140
_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)+(0.0458P)²+64.5478P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0876
_refine_ls_wR_factor_ref         0.0897
_refine_special_details          ?
_olex2_refinement_description    
;
1. Shared sites
{Dy1, Ca1}
2. Uiso/Uaniso restraints and constraints
Uanis(Dy1) = Uanis(Ca1)
3. Others
 1*[Sof(Cs1)]+1*[Sof(Cs2)]+1*[Sof(Cs3)]=0.15 with esd of 0.0001
 Fixed Sof: Dy1(0.35) Ca1(0.15)
;
_atom_sites_solution_hydrogens   .
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
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
Dy1 Dy 0.0000 0.64404(3) 0.0000 0.02165(18) Uani 0.7 2 d S T P . .
Ca1 Ca 0.0000 0.64404(3) 0.0000 0.02165(18) Uani 0.3 2 d S T P . .
S1 S 0.19398(9) 0.80602(9) 0.00078(14) 0.0320(5) Uani 1 2 d S T P . .
S2 S -0.01937(10) 0.76149(11) -0.14771(11) 0.0315(3) Uani 1 1 d . . . . .
P1 P 0.16139(8) 0.83861(8) 0.13575(14) 0.0272(4) Uani 1 2 d S T P . .
S3 S 0.08987(16) 0.54494(8) 0.08631(15) 0.0307(4) Uani 1 2 d S T P . .
Cs1 Cs 0.3333 0.6667 0.1667 0.135(3) Uani 0.817(9) 12 d S T P . .
Cs2 Cs 0.0000 1.0000 0.0000 0.213(5) Uani 0.782(12) 12 d S T P . .
Cs3 Cs 0.0000 1.0000 -0.244(6) 0.32(5) Uani 0.101(6) 6 d S T P . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
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
Dy1 S1 2.9412(4) 20_455 ?
Dy1 S1 2.9412(4) . ?
Dy1 S2 2.8734(15) . ?
Dy1 S2 2.8734(15) 6 ?
Dy1 S2 2.9040(15) 8_565 ?
Dy1 S2 2.9041(15) 16_454 ?
Dy1 S3 2.9103(12) . ?
Dy1 S3 2.9102(12) 19_565 ?
S1 Dy1 2.9412(4) 21_665 ?
S1 Ca1 2.9412(4) 21_665 ?
S1 P1 2.021(3) . ?
S1 Cs3 4.12(2) 31_564 ?
S2 Dy1 2.9041(15) 15_454 ?
S2 Ca1 2.9041(15) 15_454 ?
S2 P1 2.026(2) 20_455 ?
S2 Cs3 3.96(2) . ?
P1 Ca1 3.5332(14) 8_565 ?
P1 Ca1 3.5332(14) 26_455 ?
P1 Ca1 3.4549(10) 21_665 ?
P1 S2 2.026(2) 21_665 ?
P1 S2 2.026(2) 6 ?
P1 S3 2.053(3) 26_455 ?
S3 Dy1 2.9103(12) 19_565 ?
S3 Ca1 2.9103(12) 19_565 ?
S3 P1 2.053(3) 27 ?
S3 Cs1 3.605(2) . ?
S3 Cs3 4.16(4) 31_564 ?
Cs1 S3 3.605(2) 27 ?
Cs1 S3 3.605(2) 25_565 ?
Cs1 S3 3.605(2) 2_665 ?
Cs1 S3 3.605(2) 26_455 ?
Cs1 S3 3.605(2) 3_565 ?
Cs1 Cs3 3.41(8) 31_564 ?
Cs1 Cs3 3.41(8) 13_545 ?
Cs2 Cs3 3.25(8) 19_575 ?
Cs2 Cs3 3.25(8) . ?
Cs3 S1 4.12(2) 33_554 ?
Cs3 S1 4.12(2) 31_564 ?
Cs3 S1 4.12(2) 32_454 ?
Cs3 S2 3.96(2) 22_665 ?
Cs3 S2 3.96(2) 2_675 ?
Cs3 S2 3.96(2) 23_455 ?
Cs3 S2 3.96(2) 3_465 ?
Cs3 S2 3.96(2) 24_575 ?
Cs3 S3 4.16(4) 32_454 ?
Cs3 Cs1 3.41(8) 7_454 ?

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
S1 Dy1 S1 137.71(10) 20_455 . ?
S2 Dy1 S1 69.39(5) 6 . ?
S2 Dy1 S1 70.24(5) 8_565 20_455 ?
S2 Dy1 S1 80.25(5) . . ?
S2 Dy1 S1 70.24(5) 16_454 . ?
S2 Dy1 S1 121.15(5) 16_454 20_455 ?
S2 Dy1 S1 69.39(5) . 20_455 ?
S2 Dy1 S1 80.25(5) 6 20_455 ?
S2 Dy1 S1 121.15(5) 8_565 . ?
S2 Dy1 S2 135.93(2) . 8_565 ?
S2 Dy1 S2 151.24(6) 8_565 16_454 ?
S2 Dy1 S2 135.93(2) 6 16_454 ?
S2 Dy1 S2 68.92(5) 6 8_565 ?
S2 Dy1 S2 87.49(6) . 6 ?
S2 Dy1 S2 68.92(5) . 16_454 ?
S2 Dy1 S3 86.22(5) 8_565 19_565 ?
S2 Dy1 S3 70.40(5) 8_565 . ?
S2 Dy1 S3 105.76(5) 6 . ?
S2 Dy1 S3 86.22(5) 16_454 . ?
S2 Dy1 S3 153.65(5) . . ?
S2 Dy1 S3 105.76(5) . 19_565 ?
S2 Dy1 S3 153.65(5) 6 19_565 ?
S2 Dy1 S3 70.40(5) 16_454 19_565 ?
S3 Dy1 S1 83.27(6) 19_565 20_455 ?
S3 Dy1 S1 83.27(6) . . ?
S3 Dy1 S1 134.45(6) . 20_455 ?
S3 Dy1 S1 134.45(6) 19_565 . ?
S3 Dy1 S3 72.16(6) . 19_565 ?
Dy1 S1 Dy1 162.29(10) 21_665 . ?
Dy1 S1 Cs3 98.41(7) . 31_564 ?
Dy1 S1 Cs3 98.41(7) 21_665 31_564 ?
Ca1 S1 Dy1 0.0 21_665 21_665 ?
Ca1 S1 Dy1 162.3 21_665 . ?
Ca1 S1 Cs3 98.41(7) 21_665 31_564 ?
P1 S1 Dy1 86.15(4) . . ?
P1 S1 Dy1 86.15(4) . 21_665 ?
P1 S1 Ca1 86.15(4) . 21_665 ?
P1 S1 Cs3 134.0(10) . 31_564 ?
Dy1 S2 Dy1 101.89(5) . 15_454 ?
Dy1 S2 Ca1 101.9 . 15_454 ?
Dy1 S2 Cs3 153.8(10) . . ?
Dy1 S2 Cs3 102.6(10) 15_454 . ?
Ca1 S2 Dy1 0.0 15_454 15_454 ?
Ca1 S2 Cs3 102.6(10) 15_454 . ?
P1 S2 Dy1 87.91(7) 20_455 . ?
P1 S2 Dy1 89.73(8) 20_455 15_454 ?
P1 S2 Ca1 89.73(8) 20_455 15_454 ?
P1 S2 Cs3 101.24(8) 20_455 . ?
Ca1 P1 Ca1 79.878(10) 21_665 26_455 ?
Ca1 P1 Ca1 83.47(4) 26_455 8_565 ?
Ca1 P1 Ca1 160.77(6) 21_665 8_565 ?
S1 P1 Ca1 130.07(6) . 8_565 ?
S1 P1 Ca1 58.15(3) . 21_665 ?
S1 P1 Ca1 130.07(6) . 26_455 ?
S1 P1 S2 109.77(8) . 6 ?
S1 P1 S2 109.77(8) . 21_665 ?
S1 P1 S3 109.09(14) . 26_455 ?
S2 P1 Ca1 55.28(5) 21_665 26_455 ?
S2 P1 Ca1 55.28(5) 6 8_565 ?
S2 P1 Ca1 120.14(8) 21_665 8_565 ?
S2 P1 Ca1 120.14(8) 6 26_455 ?
S2 P1 Ca1 142.95(10) 6 21_665 ?
S2 P1 Ca1 56.22(5) 21_665 21_665 ?
S2 P1 S2 107.21(14) 21_665 6 ?
S2 P1 S3 110.49(8) 6 26_455 ?
S2 P1 S3 110.49(8) 21_665 26_455 ?
S3 P1 Ca1 55.44(5) 26_455 8_565 ?
S3 P1 Ca1 55.44(5) 26_455 26_455 ?
S3 P1 Ca1 106.50(6) 26_455 21_665 ?
Dy1 S3 Dy1 107.84(6) . 19_565 ?
Dy1 S3 Ca1 107.8 . 19_565 ?
Dy1 S3 Cs1 122.30(4) 19_565 . ?
Dy1 S3 Cs1 122.30(4) . . ?
Dy1 S3 Cs3 98.0(5) . 31_564 ?
Dy1 S3 Cs3 98.0(5) 19_565 31_564 ?
Ca1 S3 Dy1 0.0 19_565 19_565 ?
Ca1 S3 Cs1 122.30(4) 19_565 . ?
Ca1 S3 Cs3 98.0(5) 19_565 31_564 ?
P1 S3 Dy1 89.04(7) 27 19_565 ?
P1 S3 Dy1 89.03(7) 27 . ?
P1 S3 Ca1 89.04(7) 27 19_565 ?
P1 S3 Cs1 116.50(9) 27 . ?
P1 S3 Cs3 167.9(9) 27 31_564 ?
Cs1 S3 Cs3 51.4(9) . 31_564 ?
S3 Cs1 S3 180.0 3_565 27 ?
S3 Cs1 S3 111.58(3) 26_455 25_565 ?
S3 Cs1 S3 68.42(3) 3_565 25_565 ?
S3 Cs1 S3 111.58(3) 26_455 27 ?
S3 Cs1 S3 68.42(3) . 27 ?
S3 Cs1 S3 180.0 . 25_565 ?
S3 Cs1 S3 180.0 26_455 2_665 ?
S3 Cs1 S3 111.58(3) 25_565 27 ?
S3 Cs1 S3 111.58(3) . 2_665 ?
S3 Cs1 S3 111.58(3) 3_565 2_665 ?
S3 Cs1 S3 68.42(3) 27 2_665 ?
S3 Cs1 S3 68.42(3) 25_565 2_665 ?
S3 Cs1 S3 68.42(3) . 26_455 ?
S3 Cs1 S3 68.42(3) 3_565 26_455 ?
S3 Cs1 S3 111.58(3) . 3_565 ?
Cs3 Cs1 S3 72.73(3) 13_545 27 ?
Cs3 Cs1 S3 107.27(3) 31_564 25_565 ?
Cs3 Cs1 S3 107.27(3) 13_545 . ?
Cs3 Cs1 S3 107.27(3) 31_564 27 ?
Cs3 Cs1 S3 107.27(3) 13_545 3_565 ?
Cs3 Cs1 S3 72.73(3) 13_545 26_455 ?
Cs3 Cs1 S3 72.73(3) 13_545 25_565 ?
Cs3 Cs1 S3 107.27(3) 31_564 26_455 ?
Cs3 Cs1 S3 72.73(3) 31_564 . ?
Cs3 Cs1 S3 107.27(3) 13_545 2_665 ?
Cs3 Cs1 S3 72.73(3) 31_564 3_565 ?
Cs3 Cs1 S3 72.73(3) 31_564 2_665 ?
Cs3 Cs1 Cs3 180.0 13_545 31_564 ?
Cs3 Cs2 Cs3 180.0 19_575 . ?
S1 Cs3 S1 111.9(9) 33_554 31_564 ?
S1 Cs3 S1 111.9(9) 32_454 31_564 ?
S1 Cs3 S1 111.9(9) 33_554 32_454 ?
S1 Cs3 S3 56.0(5) 32_454 32_454 ?
S1 Cs3 S3 128.9(19) 31_564 32_454 ?
S1 Cs3 S3 56.0(5) 33_554 32_454 ?
S2 Cs3 S1 91.61(3) . 33_554 ?
S2 Cs3 S1 91.62(4) 2_675 31_564 ?
S2 Cs3 S1 155.38(17) 3_465 31_564 ?
S2 Cs3 S1 49.14(3) 2_675 32_454 ?
S2 Cs3 S1 91.62(4) 23_455 31_564 ?
S2 Cs3 S1 91.61(4) 22_665 32_454 ?
S2 Cs3 S1 49.14(3) . 31_564 ?
S2 Cs3 S1 155.38(17) 23_455 32_454 ?
S2 Cs3 S1 49.14(3) 22_665 31_564 ?
S2 Cs3 S1 155.38(17) 2_675 33_554 ?
S2 Cs3 S1 155.38(17) 24_575 31_564 ?
S2 Cs3 S1 155.38(17) 22_665 33_554 ?
S2 Cs3 S1 49.14(3) 23_455 33_554 ?
S2 Cs3 S1 155.38(17) . 32_454 ?
S2 Cs3 S1 49.14(3) 3_465 33_554 ?
S2 Cs3 S1 49.14(3) 24_575 32_454 ?
S2 Cs3 S1 91.62(3) 3_465 32_454 ?
S2 Cs3 S1 91.62(3) 24_575 33_554 ?
S2 Cs3 S2 110.0(10) 2_675 . ?
S2 Cs3 S2 110.0(10) 22_665 24_575 ?
S2 Cs3 S2 64.2(4) 23_455 3_465 ?
S2 Cs3 S2 64.2(5) 22_665 . ?
S2 Cs3 S2 110.0(10) 2_675 3_465 ?
S2 Cs3 S2 48.6(3) 2_675 22_665 ?
S2 Cs3 S2 64.2(4) 2_675 24_575 ?
S2 Cs3 S2 141(2) 24_575 . ?
S2 Cs3 S2 110.0(10) 23_455 24_575 ?
S2 Cs3 S2 110.0(10) 3_465 . ?
S2 Cs3 S2 141(2) 22_665 3_465 ?
S2 Cs3 S2 141(2) 2_675 23_455 ?
S2 Cs3 S2 48.6(3) 24_575 3_465 ?
S2 Cs3 S2 110.0(10) 22_665 23_455 ?
S2 Cs3 S2 48.6(3) 23_455 . ?
S2 Cs3 S3 146.1(8) . 32_454 ?
S2 Cs3 S3 58.52(19) 24_575 32_454 ?
S2 Cs3 S3 103.9(3) 23_455 32_454 ?
S2 Cs3 S3 58.52(19) 3_465 32_454 ?
S2 Cs3 S3 146.1(8) 22_665 32_454 ?
S2 Cs3 S3 103.9(3) 2_675 32_454 ?
Cs1 Cs3 S1 73.1(10) 7_454 31_564 ?
Cs1 Cs3 S1 73.1(10) 7_454 33_554 ?
Cs1 Cs3 S1 73.1(10) 7_454 32_454 ?
Cs1 Cs3 S2 108.9(10) 7_454 3_465 ?
Cs1 Cs3 S2 108.9(10) 7_454 . ?
Cs1 Cs3 S2 108.9(10) 7_454 24_575 ?
Cs1 Cs3 S2 108.9(10) 7_454 22_665 ?
Cs1 Cs3 S2 108.9(10) 7_454 2_675 ?
Cs1 Cs3 S2 108.9(10) 7_454 23_455 ?
Cs1 Cs3 S3 55.8(9) 7_454 32_454 ?
Cs2 Cs3 S1 106.9(10) . 32_454 ?
Cs2 Cs3 S1 106.9(10) . 31_564 ?
Cs2 Cs3 S1 106.9(10) . 33_554 ?
Cs2 Cs3 S2 71.1(10) . . ?
Cs2 Cs3 S2 71.1(10) . 23_455 ?
Cs2 Cs3 S2 71.1(10) . 3_465 ?
Cs2 Cs3 S2 71.1(10) . 22_665 ?
Cs2 Cs3 S2 71.1(10) . 2_675 ?
Cs2 Cs3 S2 71.1(10) . 24_575 ?
Cs2 Cs3 S3 124.2(9) . 32_454 ?
Cs2 Cs3 Cs1 180.0 . 7_454 ?


# start Validation Reply Form
_vrf_PLAT971_1                   
;
PROBLEM: Check Calcd Resid. Dens.  0.84A   From Cs2             3.68 eA-3  
RESPONSE: The cesium atoms are severely disordered along the channels in
the structure and cannot be located from the difference map. Due to this
they have been resolved as residing at three positions with overall 
occupancy equal to 0.15 to accomplish charge balance.
;
_vrf_PLAT974_1                   
;
PROBLEM: Check Calcd Negative Resid. Density on       Cs2      -3.92 eA-3  
RESPONSE: The cesium atoms are severely disordered along the channels in
the structure and cannot be located from the difference map. Due to this
they have been resolved as residing at three positions with overall 
occupancy equal to 0.15 to accomplish charge balance.
;
_vrf_PLAT214_1                   
;
PROBLEM: Atom Cs3       (Anion/Solvent) ADP max/min Ratio        5.9 prolat
RESPONSE: The cesium atoms are severely disordered along the channels in
the structure and cannot be located from the difference map. Due to this
they have been resolved as residing at three positions with overall 
occupancy equal to 0.15 to accomplish charge balance.
;
_vrf_PLAT260_1                   
;
PROBLEM: Large Average Ueq of Residue Including       Cs3      0.318 Check 
RESPONSE: The cesium atoms are severely disordered along the channels in
the structure and cannot be located from the difference map. Due to this
they have been resolved as residing at three positions with overall 
occupancy equal to 0.15 to accomplish charge balance.
;
_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_Tb07
_database_code_depnum_ccdc_archive 'CCDC 2038463'
loop_
_audit_author_name
_audit_author_address
'Vladislav Klepov'
;University of South Carolina
United States of America
;
_audit_update_record             
;
2020-10-14 deposited with the CCDC.	2020-12-01 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/1
_shelx_SHELXL_version_number     2018/1
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'Ca0.30 Cs0.30 P S4 Tb0.70'
_chemical_formula_weight         322.35

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Ca Ca 0.2262 0.3064 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cs Cs -0.3680 2.1192 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Tb Tb -0.1723 4.1537 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 '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'

_space_group_crystal_system      trigonal
_space_group_IT_number           166
_space_group_name_H-M_alt        'R -3 m :H'
_space_group_name_Hall           '-R 3 2"'

_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.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'y, x, -z'
'x-y, -y, -z'
'-x, -x+y, -z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'y+2/3, x+1/3, -z+1/3'
'x-y+2/3, -y+1/3, -z+1/3'
'-x+2/3, -x+y+1/3, -z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'y+1/3, x+2/3, -z+2/3'
'x-y+1/3, -y+2/3, -z+2/3'
'-x+1/3, -x+y+2/3, -z+2/3'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-y, -x, z'
'-x+y, y, z'
'x, x-y, z'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-y+2/3, -x+1/3, z+1/3'
'-x+y+2/3, y+1/3, z+1/3'
'x+2/3, x-y+1/3, z+1/3'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'
'-y+1/3, -x+2/3, z+2/3'
'-x+y+1/3, y+2/3, z+2/3'
'x+1/3, x-y+2/3, z+2/3'

_cell_length_a                   16.3448(4)
_cell_length_b                   16.3448(4)
_cell_length_c                   13.3425(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     3086.93(17)
_cell_formula_units_Z            18
_cell_measurement_temperature    300(2)
_cell_measurement_reflns_used    9404
_cell_measurement_theta_min      3.26
_cell_measurement_theta_max      33.11

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    3.121
_exptl_crystal_F_000             2646
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.030
_exptl_crystal_size_mid          0.020
_exptl_crystal_size_min          0.020
_exptl_absorpt_coefficient_mu    10.379
_shelx_estimated_absorpt_T_min   0.746
_shelx_estimated_absorpt_T_max   0.819
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.2210
_exptl_absorpt_correction_T_max  0.2694
_exptl_absorpt_process_details   
;
 Reference: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D.,
 J. Appl. Cryst. 48 (2015) 3-10.
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      300(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker D8 QUEST'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            30233
_diffrn_reflns_av_unetI/netI     0.0069
_diffrn_reflns_av_R_equivalents  0.0243
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         3.258
_diffrn_reflns_theta_max         27.499
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measured_fraction_theta_full 0.987
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_Laue_measured_fraction_full 0.987
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_point_group_measured_fraction_full 0.987
_reflns_number_total             875
_reflns_number_gt                874
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2018/1 (Sheldrick, 2018)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0492P)²+54.2359P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   .
_refine_ls_hydrogen_treatment    undef
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         875
_refine_ls_number_parameters     43
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0298
_refine_ls_R_factor_gt           0.0298
_refine_ls_wR_factor_ref         0.0878
_refine_ls_wR_factor_gt          0.0878
_refine_ls_goodness_of_fit_ref   1.126
_refine_ls_restrained_S_all      1.126
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

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
Tb1 Tb 0.000000 0.64423(2) 0.000000 0.02042(18) Uani 0.7 2 d S T P . .
Ca1 Ca 0.000000 0.64423(2) 0.000000 0.02042(18) Uani 0.3 2 d S T P . .
S1 S 0.19379(8) 0.80621(8) 0.00099(12) 0.0321(4) Uani 1 2 d S T P . .
S2 S -0.01934(9) 0.76184(10) -0.14780(9) 0.0304(3) Uani 1 1 d . . . . .
P1 P 0.16110(8) 0.83890(8) 0.13586(12) 0.0266(4) Uani 1 2 d S T P . .
S3 S 0.08948(14) 0.54474(7) 0.08679(14) 0.0292(4) Uani 1 2 d S T P . .
Cs1 Cs 0.333333 0.666667 0.166667 0.1136(19) Uani 0.860(9) 12 d S T P . .
Cs2 Cs 0.000000 1.000000 0.000000 0.206(4) Uani 0.852(12) 12 d S T P . .
Cs3 Cs 0.000000 1.000000 -0.239(14) 0.50(16) Uani 0.044(6) 6 d S T P . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

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
Tb1 S2 2.8795(13) 6 ?
Tb1 S2 2.8796(13) . ?
Tb1 S2 2.9107(13) 8_565 ?
Tb1 S2 2.9107(13) 16_454 ?
Tb1 S3 2.9159(11) 19_565 ?
Tb1 S3 2.9159(11) . ?
Tb1 S1 2.9422(4) . ?
Tb1 S1 2.9422(4) 20_455 ?
S1 P1 2.024(2) . ?
S1 Cs3 4.15(6) 31_564 ?
S2 P1 2.0244(18) 20_455 ?
S2 Cs3 3.94(6) . ?
P1 S3 2.052(3) 26_455 ?
S3 Cs1 3.6125(18) . ?
Cs1 Cs3 3.49(19) 13_545 ?
Cs1 Cs3 3.49(19) 31_564 ?
Cs2 Cs3 3.18(19) . ?
Cs2 Cs3 3.18(19) 19_575 ?

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
S2 Tb1 S2 87.48(6) 6 . ?
S2 Tb1 S2 69.02(4) 6 8_565 ?
S2 Tb1 S2 135.97(2) . 8_565 ?
S2 Tb1 S2 135.97(2) 6 16_454 ?
S2 Tb1 S2 69.03(4) . 16_454 ?
S2 Tb1 S2 151.06(5) 8_565 16_454 ?
S2 Tb1 S3 153.81(5) 6 19_565 ?
S2 Tb1 S3 105.71(4) . 19_565 ?
S2 Tb1 S3 86.26(5) 8_565 19_565 ?
S2 Tb1 S3 70.20(5) 16_454 19_565 ?
S2 Tb1 S3 105.71(4) 6 . ?
S2 Tb1 S3 153.81(5) . . ?
S2 Tb1 S3 70.20(5) 8_565 . ?
S2 Tb1 S3 86.26(5) 16_454 . ?
S3 Tb1 S3 72.11(6) 19_565 . ?
S2 Tb1 S1 69.33(4) 6 . ?
S2 Tb1 S1 80.24(5) . . ?
S2 Tb1 S1 121.20(4) 8_565 . ?
S2 Tb1 S1 70.28(4) 16_454 . ?
S3 Tb1 S1 134.35(5) 19_565 . ?
S3 Tb1 S1 83.43(6) . . ?
S2 Tb1 S1 80.24(5) 6 20_455 ?
S2 Tb1 S1 69.33(4) . 20_455 ?
S2 Tb1 S1 70.28(4) 8_565 20_455 ?
S2 Tb1 S1 121.20(4) 16_454 20_455 ?
S3 Tb1 S1 83.43(6) 19_565 20_455 ?
S3 Tb1 S1 134.35(5) . 20_455 ?
S1 Tb1 S1 137.61(9) . 20_455 ?
P1 S1 Tb1 86.21(3) . . ?
P1 S1 Tb1 86.21(3) . 21_665 ?
Tb1 S1 Tb1 162.38(9) . 21_665 ?
P1 S1 Cs3 135(3) . 31_564 ?
Tb1 S1 Cs3 98.30(14) . 31_564 ?
Tb1 S1 Cs3 98.29(15) 21_665 31_564 ?
P1 S2 Tb1 87.91(6) 20_455 . ?
P1 S2 Tb1 89.78(7) 20_455 15_454 ?
Tb1 S2 Tb1 101.77(4) . 15_454 ?
P1 S2 Cs3 101.19(9) 20_455 . ?
Tb1 S2 Cs3 153(3) . . ?
Tb1 S2 Cs3 104(3) 15_454 . ?
S1 P1 S2 109.80(7) . 21_665 ?
S1 P1 S2 109.80(7) . 6 ?
S2 P1 S2 107.28(12) 21_665 6 ?
S1 P1 S3 108.82(13) . 26_455 ?
S2 P1 S3 110.56(7) 21_665 26_455 ?
S2 P1 S3 110.56(7) 6 26_455 ?
S1 P1 Ca1 129.92(6) . 26_455 ?
S2 P1 Ca1 55.33(5) 21_665 26_455 ?
S2 P1 Ca1 120.26(7) 6 26_455 ?
S3 P1 Ca1 55.47(4) 26_455 26_455 ?
S1 P1 Ca1 129.92(6) . 8_565 ?
S2 P1 Ca1 120.26(7) 21_665 8_565 ?
S2 P1 Ca1 55.33(5) 6 8_565 ?
S3 P1 Ca1 55.47(4) 26_455 8_565 ?
Ca1 P1 Ca1 83.54(4) 26_455 8_565 ?
P1 S3 Tb1 89.11(6) 27 19_565 ?
P1 S3 Tb1 89.10(6) 27 . ?
Tb1 S3 Tb1 107.89(6) 19_565 . ?
P1 S3 Cs1 116.80(8) 27 . ?
Tb1 S3 Cs1 122.15(4) 19_565 . ?
Tb1 S3 Cs1 122.15(4) . . ?
Cs3 Cs1 Cs3 180.0 13_545 31_564 ?
Cs3 Cs1 S3 72.84(3) 13_545 25_565 ?
Cs3 Cs1 S3 107.16(3) 31_564 25_565 ?
Cs3 Cs1 S3 72.84(3) 13_545 27 ?
Cs3 Cs1 S3 107.16(3) 31_564 27 ?
S3 Cs1 S3 111.68(3) 25_565 27 ?
Cs3 Cs1 S3 107.16(3) 13_545 . ?
Cs3 Cs1 S3 72.84(3) 31_564 . ?
S3 Cs1 S3 180.0 25_565 . ?
S3 Cs1 S3 68.32(3) 27 . ?
Cs3 Cs1 S3 107.16(3) 13_545 3_565 ?
Cs3 Cs1 S3 72.84(3) 31_564 3_565 ?
S3 Cs1 S3 68.32(3) 25_565 3_565 ?
S3 Cs1 S3 180.0 27 3_565 ?
S3 Cs1 S3 111.68(3) . 3_565 ?
Cs3 Cs1 S3 107.16(3) 13_545 2_665 ?
Cs3 Cs1 S3 72.84(3) 31_564 2_665 ?
S3 Cs1 S3 68.32(3) 25_565 2_665 ?
S3 Cs1 S3 68.32(3) 27 2_665 ?
S3 Cs1 S3 111.68(3) . 2_665 ?
S3 Cs1 S3 111.68(3) 3_565 2_665 ?
Cs3 Cs1 S3 72.84(3) 13_545 26_455 ?
Cs3 Cs1 S3 107.16(3) 31_564 26_455 ?
S3 Cs1 S3 111.68(3) 25_565 26_455 ?
S3 Cs1 S3 111.68(3) 27 26_455 ?
S3 Cs1 S3 68.32(3) . 26_455 ?
S3 Cs1 S3 68.32(3) 3_565 26_455 ?
S3 Cs1 S3 180.0 2_665 26_455 ?
Cs3 Cs2 Cs3 180.00(2) . 19_575 ?
Cs2 Cs3 Cs1 180.0 . 7_454 ?
Cs2 Cs3 S2 72(3) . . ?
Cs1 Cs3 S2 108(3) 7_454 . ?
Cs2 Cs3 S2 72(3) . 2_675 ?
Cs1 Cs3 S2 108(3) 7_454 2_675 ?
S2 Cs3 S2 111(2) . 2_675 ?
Cs2 Cs3 S2 72(3) . 22_665 ?
Cs1 Cs3 S2 108(3) 7_454 22_665 ?
S2 Cs3 S2 64.6(11) . 22_665 ?
S2 Cs3 S2 48.9(8) 2_675 22_665 ?
Cs2 Cs3 S2 72(3) . 23_455 ?
Cs1 Cs3 S2 108(3) 7_454 23_455 ?
S2 Cs3 S2 48.9(8) . 23_455 ?
S2 Cs3 S2 143(5) 2_675 23_455 ?
S2 Cs3 S2 111(2) 22_665 23_455 ?
Cs2 Cs3 S2 72(3) . 24_575 ?
Cs1 Cs3 S2 108(3) 7_454 24_575 ?
S2 Cs3 S2 143(5) . 24_575 ?
S2 Cs3 S2 64.6(11) 2_675 24_575 ?
S2 Cs3 S2 111(2) 22_665 24_575 ?
S2 Cs3 S2 111(2) 23_455 24_575 ?
Cs2 Cs3 S2 72(3) . 3_465 ?
Cs1 Cs3 S2 108(3) 7_454 3_465 ?
S2 Cs3 S2 111(2) . 3_465 ?
S2 Cs3 S2 111(2) 2_675 3_465 ?
S2 Cs3 S2 143(5) 22_665 3_465 ?
S2 Cs3 S2 64.6(11) 23_455 3_465 ?
S2 Cs3 S2 48.9(8) 24_575 3_465 ?
Cs2 Cs3 S1 108(2) . 33_554 ?
Cs1 Cs3 S1 72(2) 7_454 33_554 ?
S2 Cs3 S1 91.63(5) . 33_554 ?
S2 Cs3 S1 155.47(2) 2_675 33_554 ?
S2 Cs3 S1 155.46(2) 22_665 33_554 ?
S2 Cs3 S1 49.15(10) 23_455 33_554 ?
S2 Cs3 S1 91.64(5) 24_575 33_554 ?
S2 Cs3 S1 49.15(10) 3_465 33_554 ?
Cs2 Cs3 S1 108(2) . 32_454 ?
Cs1 Cs3 S1 72(2) 7_454 32_454 ?
S2 Cs3 S1 155.46(2) . 32_454 ?
S2 Cs3 S1 49.15(10) 2_675 32_454 ?
S2 Cs3 S1 91.63(5) 22_665 32_454 ?
S2 Cs3 S1 155.47(2) 23_455 32_454 ?
S2 Cs3 S1 49.15(10) 24_575 32_454 ?
S2 Cs3 S1 91.64(5) 3_465 32_454 ?
S1 Cs3 S1 111(2) 33_554 32_454 ?
Cs2 Cs3 S1 108(2) . 31_564 ?
Cs1 Cs3 S1 72(2) 7_454 31_564 ?
S2 Cs3 S1 49.15(10) . 31_564 ?
S2 Cs3 S1 91.63(5) 2_675 31_564 ?
S2 Cs3 S1 49.15(10) 22_665 31_564 ?
S2 Cs3 S1 91.63(5) 23_455 31_564 ?
S2 Cs3 S1 155.47(2) 24_575 31_564 ?
S2 Cs3 S1 155.46(2) 3_465 31_564 ?
S1 Cs3 S1 111(2) 33_554 31_564 ?
S1 Cs3 S1 111(2) 32_454 31_564 ?

_refine_diff_density_max         3.038
_refine_diff_density_min         -4.245
_refine_diff_density_rms         0.187



# start Validation Reply Form
_vrf_PLAT214_1                   
;
PROBLEM: Atom Cs3       (Anion/Solvent) ADP max/min Ratio       15.0 prolat
RESPONSE: The cesium atoms are severely disordered along the channels in
the structure and cannot be located from the difference map. Due to this
they have been resolved as residing at three positions with overall 
occupancy equal to 0.15 to accomplish charge balance.
;
_vrf_PLAT974_1                   
;
PROBLEM: Check Calcd Negative Resid. Density on       Cs2      -4.40 eA-3  
RESPONSE: The cesium atoms are severely disordered along the channels in
the structure and cannot be located from the difference map. Due to this
they have been resolved as residing at three positions with overall 
occupancy equal to 0.15 to accomplish charge balance.
;
_vrf_PLAT260_1                   
;
PROBLEM: Large Average Ueq of Residue Including       Cs3      0.505 Check 
RESPONSE: The cesium atoms are severely disordered along the channels in
the structure and cannot be located from the difference map. Due to this
they have been resolved as residing at three positions with overall 
occupancy equal to 0.15 to accomplish charge balance.
;
_vrf_PLAT971_1                   
;
PROBLEM: Check Calcd Resid. Dens.  0.84A   From Cs2             2.97 eA-3  
RESPONSE: The cesium atoms are severely disordered along the channels in
the structure and cannot be located from the difference map. Due to this
they have been resolved as residing at three positions with overall 
occupancy equal to 0.15 to accomplish charge balance.
;
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_Sm05
_database_code_depnum_ccdc_archive 'CCDC 2038467'
loop_
_audit_author_name
_audit_author_address
'Vladislav Klepov'
;University of South Carolina
United States of America
;
_audit_update_record             
;
2020-10-14 deposited with the CCDC.	2020-12-01 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/1
_shelx_SHELXL_version_number     2018/1
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'Ca0.50 Cs0.50 P S4 Sm0.50'
_chemical_formula_weight         320.88

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
P P 0.1023 0.0942 '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'
Ca Ca 0.2262 0.3064 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cs Cs -0.3680 2.1192 '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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 2/c'
_space_group_name_Hall           '-C 2yc'

_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.
;

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'

_cell_length_a                   9.1778(3)
_cell_length_b                   9.2037(3)
_cell_length_c                   16.6857(5)
_cell_angle_alpha                90
_cell_angle_beta                 103.7780(13)
_cell_angle_gamma                90
_cell_volume                     1368.88(8)
_cell_formula_units_Z            8
_cell_measurement_temperature    300(2)
_cell_measurement_reflns_used    9134
_cell_measurement_theta_min      2.51
_cell_measurement_theta_max      33.11

_exptl_crystal_description       plate
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    3.114
_exptl_crystal_F_000             1180
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.060
_exptl_crystal_size_mid          0.040
_exptl_crystal_size_min          0.010
_exptl_absorpt_coefficient_mu    8.692
_shelx_estimated_absorpt_T_min   0.624
_shelx_estimated_absorpt_T_max   0.918
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.1734
_exptl_absorpt_correction_T_max  0.2694
_exptl_absorpt_process_details   
;
 Reference: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D.,
 J. Appl. Cryst. 48 (2015) 3-10.
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      300(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker D8 QUEST'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            19807
_diffrn_reflns_av_unetI/netI     0.0185
_diffrn_reflns_av_R_equivalents  0.0360
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         2.514
_diffrn_reflns_theta_max         29.995
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             1989
_reflns_number_gt                1882
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2018/1 (Sheldrick, 2018)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0135P)²+8.3031P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   .
_refine_ls_hydrogen_treatment    undef
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         1989
_refine_ls_number_parameters     60
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0247
_refine_ls_R_factor_gt           0.0231
_refine_ls_wR_factor_ref         0.0534
_refine_ls_wR_factor_gt          0.0526
_refine_ls_goodness_of_fit_ref   1.098
_refine_ls_restrained_S_all      1.098
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

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
Cs1 Cs 0.000000 0.64326(3) 0.250000 0.03386(8) Uani 1 2 d S T P . .
Sm1 Sm 0.49361(3) 0.73193(3) 0.02445(2) 0.02647(7) Uani 0.5 1 d . . P . .
Ca1 Ca 0.49361(3) 0.73193(3) 0.02445(2) 0.02647(7) Uani 0.5 1 d . . P . .
P1 P 0.27516(8) 0.48524(8) 0.09191(5) 0.02021(14) Uani 1 1 d . . . . .
S1 S 0.25231(9) 0.70168(8) 0.11122(5) 0.02748(16) Uani 1 1 d . . . . .
S2 S 0.18183(9) 0.36052(8) 0.16538(5) 0.02574(15) Uani 1 1 d . . . . .
S3 S 0.50072(9) 0.45439(9) 0.11160(5) 0.02796(16) Uani 1 1 d . . . . .
S4 S 0.17965(13) 0.44193(12) -0.02995(5) 0.0460(3) Uani 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

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
Cs1 S2 3.5433(8) 4 ?
Cs1 S2 3.5433(8) 3_455 ?
Cs1 S2 3.5598(8) 2 ?
Cs1 S2 3.5598(8) . ?
Cs1 S3 3.6797(8) 4 ?
Cs1 S3 3.6797(8) 3_455 ?
Cs1 S1 3.6834(8) . ?
Cs1 S1 3.6834(8) 2 ?
Cs1 S4 3.7324(9) 5_565 ?
Cs1 S4 3.7324(9) 6_566 ?
Cs1 Sm1 4.7352(3) 8_466 ?
Cs1 Sm1 4.7352(3) 7_565 ?
Ca1 S2 2.8248(8) 3 ?
Ca1 S3 2.8554(9) 5_665 ?
Ca1 S1 2.8563(9) 7_565 ?
Ca1 S4 2.8659(9) 3 ?
Ca1 S3 2.9323(8) . ?
Ca1 S1 2.9335(8) . ?
Ca1 S4 3.3809(14) 5_665 ?
Ca1 P1 3.3935(7) . ?
Ca1 S4 3.4084(13) 7_565 ?
Ca1 P1 3.4633(8) 3 ?
P1 S2 2.0136(10) . ?
P1 S1 2.0367(10) . ?
P1 S3 2.0372(10) . ?
P1 S4 2.0525(11) . ?

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
S2 Cs1 S2 111.29(3) 4 3_455 ?
S2 Cs1 S2 132.39(2) 4 2 ?
S2 Cs1 S2 98.678(9) 3_455 2 ?
S2 Cs1 S2 98.677(9) 4 . ?
S2 Cs1 S2 132.39(2) 3_455 . ?
S2 Cs1 S2 86.06(2) 2 . ?
S2 Cs1 S3 55.615(17) 4 4 ?
S2 Cs1 S3 71.724(19) 3_455 4 ?
S2 Cs1 S3 104.411(17) 2 4 ?
S2 Cs1 S3 152.731(18) . 4 ?
S2 Cs1 S3 71.724(19) 4 3_455 ?
S2 Cs1 S3 55.615(17) 3_455 3_455 ?
S2 Cs1 S3 152.731(18) 2 3_455 ?
S2 Cs1 S3 104.412(17) . 3_455 ?
S3 Cs1 S3 77.81(3) 4 3_455 ?
S2 Cs1 S1 65.562(18) 4 . ?
S2 Cs1 S1 104.415(17) 3_455 . ?
S2 Cs1 S1 141.291(18) 2 . ?
S2 Cs1 S1 55.465(16) . . ?
S3 Cs1 S1 112.104(18) 4 . ?
S3 Cs1 S1 52.879(17) 3_455 . ?
S2 Cs1 S1 104.415(17) 4 2 ?
S2 Cs1 S1 65.562(18) 3_455 2 ?
S2 Cs1 S1 55.465(16) 2 2 ?
S2 Cs1 S1 141.291(18) . 2 ?
S3 Cs1 S1 52.879(17) 4 2 ?
S3 Cs1 S1 112.104(18) 3_455 2 ?
S1 Cs1 S1 163.21(2) . 2 ?
S2 Cs1 S4 129.761(19) 4 5_565 ?
S2 Cs1 S4 66.27(2) 3_455 5_565 ?
S2 Cs1 S4 95.603(19) 2 5_565 ?
S2 Cs1 S4 66.13(2) . 5_565 ?
S3 Cs1 S4 135.60(2) 4 5_565 ?
S3 Cs1 S4 67.20(2) 3_455 5_565 ?
S1 Cs1 S4 66.97(2) . 5_565 ?
S1 Cs1 S4 116.91(2) 2 5_565 ?
S2 Cs1 S4 66.27(2) 4 6_566 ?
S2 Cs1 S4 129.761(18) 3_455 6_566 ?
S2 Cs1 S4 66.13(2) 2 6_566 ?
S2 Cs1 S4 95.602(19) . 6_566 ?
S3 Cs1 S4 67.20(2) 4 6_566 ?
S3 Cs1 S4 135.60(2) 3_455 6_566 ?
S1 Cs1 S4 116.91(2) . 6_566 ?
S1 Cs1 S4 66.97(2) 2 6_566 ?
S4 Cs1 S4 155.75(4) 5_565 6_566 ?
S2 Cs1 Sm1 71.130(13) 4 8_466 ?
S2 Cs1 Sm1 92.843(13) 3_455 8_466 ?
S2 Cs1 Sm1 71.265(12) 2 8_466 ?
S2 Cs1 Sm1 132.521(13) . 8_466 ?
S3 Cs1 Sm1 37.060(13) 4 8_466 ?
S3 Cs1 Sm1 114.861(15) 3_455 8_466 ?
S1 Cs1 Sm1 136.636(14) . 8_466 ?
S1 Cs1 Sm1 37.076(13) 2 8_466 ?
S4 Cs1 Sm1 153.897(19) 5_565 8_466 ?
S4 Cs1 Sm1 37.242(14) 6_566 8_466 ?
S2 Cs1 Sm1 92.843(13) 4 7_565 ?
S2 Cs1 Sm1 71.130(13) 3_455 7_565 ?
S2 Cs1 Sm1 132.522(13) 2 7_565 ?
S2 Cs1 Sm1 71.266(12) . 7_565 ?
S3 Cs1 Sm1 114.861(15) 4 7_565 ?
S3 Cs1 Sm1 37.060(13) 3_455 7_565 ?
S1 Cs1 Sm1 37.076(13) . 7_565 ?
S1 Cs1 Sm1 136.636(14) 2 7_565 ?
S4 Cs1 Sm1 37.242(14) 5_565 7_565 ?
S4 Cs1 Sm1 153.897(19) 6_566 7_565 ?
Sm1 Cs1 Sm1 151.920(10) 8_466 7_565 ?
S2 Ca1 S3 142.20(2) 3 5_665 ?
S2 Ca1 S1 141.38(2) 3 7_565 ?
S3 Ca1 S1 70.06(2) 5_665 7_565 ?
S2 Ca1 S4 71.87(2) 3 3 ?
S3 Ca1 S4 91.61(3) 5_665 3 ?
S1 Ca1 S4 91.30(3) 7_565 3 ?
S2 Ca1 S3 90.87(2) 3 . ?
S3 Ca1 S3 82.45(3) 5_665 . ?
S1 Ca1 S3 119.97(2) 7_565 . ?
S4 Ca1 S3 143.13(3) 3 . ?
S2 Ca1 S1 90.73(2) 3 . ?
S3 Ca1 S1 119.62(2) 5_665 . ?
S1 Ca1 S1 82.22(3) 7_565 . ?
S4 Ca1 S1 142.85(3) 3 . ?
S3 Ca1 S1 66.60(2) . . ?
S2 Ca1 S4 79.23(2) 3 5_665 ?
S3 Ca1 S4 63.47(2) 5_665 5_665 ?
S1 Ca1 S4 130.63(2) 7_565 5_665 ?
S4 Ca1 S4 74.71(4) 3 5_665 ?
S3 Ca1 S4 70.09(2) . 5_665 ?
S1 Ca1 S4 135.29(2) . 5_665 ?
S2 Ca1 P1 107.26(2) 3 . ?
S3 Ca1 P1 89.20(2) 5_665 . ?
S1 Ca1 P1 89.33(2) 7_565 . ?
S4 Ca1 P1 179.11(2) 3 . ?
S3 Ca1 P1 36.664(19) . . ?
S1 Ca1 P1 36.652(19) . . ?
S4 Ca1 P1 105.34(2) 5_665 . ?
S2 Ca1 S4 78.77(2) 3 7_565 ?
S3 Ca1 S4 130.34(2) 5_665 7_565 ?
S1 Ca1 S4 63.08(2) 7_565 7_565 ?
S4 Ca1 S4 74.43(4) 3 7_565 ?
S3 Ca1 S4 135.18(2) . 7_565 ?
S1 Ca1 S4 70.03(2) . 7_565 ?
S4 Ca1 S4 146.36(3) 5_665 7_565 ?
P1 Ca1 S4 105.31(2) . 7_565 ?
S2 Ca1 P1 35.549(19) 3 3 ?
S3 Ca1 P1 120.61(2) 5_665 3 ?
S1 Ca1 P1 120.08(2) 7_565 3 ?
S4 Ca1 P1 36.32(2) 3 3 ?
S3 Ca1 P1 119.90(2) . 3 ?
S1 Ca1 P1 119.74(2) . 3 ?
S4 Ca1 P1 73.83(2) 5_665 3 ?
P1 Ca1 P1 142.81(2) . 3 ?
S4 Ca1 P1 73.45(2) 7_565 3 ?
S2 Ca1 Cs1 123.879(16) 3 7_565 ?
S3 Ca1 Cs1 50.953(17) 5_665 7_565 ?
S1 Ca1 Cs1 51.028(17) 7_565 7_565 ?
S4 Ca1 Cs1 52.013(18) 3 7_565 ?
S3 Ca1 Cs1 133.392(18) . 7_565 ?
S1 Ca1 Cs1 133.238(18) . 7_565 ?
S4 Ca1 Cs1 85.749(16) 5_665 7_565 ?
P1 Ca1 Cs1 128.863(15) . 7_565 ?
S4 Ca1 Cs1 85.739(16) 7_565 7_565 ?
P1 Ca1 Cs1 88.330(13) 3 7_565 ?
S2 P1 S1 112.74(5) . . ?
S2 P1 S3 112.68(5) . . ?
S1 P1 S3 104.46(5) . . ?
S2 P1 S4 110.44(5) . . ?
S1 P1 S4 108.12(5) . . ?
S3 P1 S4 108.09(5) . . ?
S2 P1 Ca1 162.54(4) . . ?
S1 P1 Ca1 59.29(3) . . ?
S3 P1 Ca1 59.26(3) . . ?
S4 P1 Ca1 87.02(3) . . ?
P1 S1 Sm1 100.11(4) . 7_565 ?
P1 S1 Ca1 84.06(3) . . ?
Sm1 S1 Ca1 97.78(3) 7_565 . ?
P1 S1 Cs1 93.47(3) . . ?
Sm1 S1 Cs1 91.90(2) 7_565 . ?
Ca1 S1 Cs1 170.29(3) . . ?
P1 S2 Sm1 89.80(3) . 3_445 ?
P1 S2 Cs1 97.74(3) . 3_545 ?
Sm1 S2 Cs1 112.20(2) 3_445 3_545 ?
P1 S2 Cs1 97.60(3) . . ?
Sm1 S2 Cs1 112.64(2) 3_445 . ?
Cs1 S2 Cs1 132.39(2) 3_545 . ?
P1 S3 Sm1 99.54(4) . 5_665 ?
P1 S3 Ca1 84.08(3) . . ?
Sm1 S3 Ca1 97.55(3) 5_665 . ?
P1 S3 Cs1 93.21(3) . 3_545 ?
Sm1 S3 Cs1 91.99(2) 5_665 3_545 ?
Ca1 S3 Cs1 170.39(3) . 3_545 ?
P1 S4 Sm1 87.90(4) . 3_445 ?
P1 S4 Cs1 178.64(4) . 5_565 ?
Sm1 S4 Cs1 90.75(2) 3_445 5_565 ?

_refine_diff_density_max         0.884
_refine_diff_density_min         -1.004
_refine_diff_density_rms         0.116

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_Nd07
_database_code_depnum_ccdc_archive 'CCDC 2038460'
loop_
_audit_author_name
_audit_author_address
'Vladislav Klepov'
;University of South Carolina
United States of America
;
_audit_update_record             
;
2020-10-14 deposited with the CCDC.	2020-12-01 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/1
_shelx_SHELXL_version_number     2018/1
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'Ca0.30 Cs0.30 Nd0.70 P S4'
_chemical_formula_weight         312.08

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Ca Ca 0.2262 0.3064 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cs Cs -0.3680 2.1192 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Nd Nd -0.1943 3.0179 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 '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'

_space_group_crystal_system      trigonal
_space_group_IT_number           166
_space_group_name_H-M_alt        'R -3 m :H'
_space_group_name_Hall           '-R 3 2"'

_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.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'y, x, -z'
'x-y, -y, -z'
'-x, -x+y, -z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'y+2/3, x+1/3, -z+1/3'
'x-y+2/3, -y+1/3, -z+1/3'
'-x+2/3, -x+y+1/3, -z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'y+1/3, x+2/3, -z+2/3'
'x-y+1/3, -y+2/3, -z+2/3'
'-x+1/3, -x+y+2/3, -z+2/3'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-y, -x, z'
'-x+y, y, z'
'x, x-y, z'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-y+2/3, -x+1/3, z+1/3'
'-x+y+2/3, y+1/3, z+1/3'
'x+2/3, x-y+1/3, z+1/3'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'
'-y+1/3, -x+2/3, z+2/3'
'-x+y+1/3, y+2/3, z+2/3'
'x+1/3, x-y+2/3, z+2/3'

_cell_length_a                   16.4932(4)
_cell_length_b                   16.4932(4)
_cell_length_c                   13.5289(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     3187.15(17)
_cell_formula_units_Z            18
_cell_measurement_temperature    300(2)
_cell_measurement_reflns_used    9811
_cell_measurement_theta_min      2.47
_cell_measurement_theta_max      33.09

_exptl_crystal_description       block
_exptl_crystal_colour            blue
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.927
_exptl_crystal_F_000             2583
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.050
_exptl_crystal_size_mid          0.040
_exptl_crystal_size_min          0.040
_exptl_absorpt_coefficient_mu    8.194
_shelx_estimated_absorpt_T_min   0.685
_shelx_estimated_absorpt_T_max   0.735
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.4524
_exptl_absorpt_correction_T_max  0.4954
_exptl_absorpt_process_details   
;
 Reference: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D.,
 J. Appl. Cryst. 48 (2015) 3-10.
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      300(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker D8 QUEST'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            32476
_diffrn_reflns_av_unetI/netI     0.0063
_diffrn_reflns_av_R_equivalents  0.0247
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         3.226
_diffrn_reflns_theta_max         27.485
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measured_fraction_theta_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_point_group_measured_fraction_full 0.994
_reflns_number_total             906
_reflns_number_gt                898
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2018/1 (Sheldrick, 2018)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0492P)²+54.2359P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   .
_refine_ls_hydrogen_treatment    undef
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         906
_refine_ls_number_parameters     44
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0332
_refine_ls_R_factor_gt           0.0330
_refine_ls_wR_factor_ref         0.0924
_refine_ls_wR_factor_gt          0.0922
_refine_ls_goodness_of_fit_ref   1.161
_refine_ls_restrained_S_all      1.161
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

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
Nd1 Nd 0.000000 0.64475(3) 0.000000 0.01947(18) Uani 0.7 2 d S T P . .
Ca1 Ca 0.000000 0.64475(3) 0.000000 0.01947(18) Uani 0.3 2 d S T P . .
S1 S 0.19252(8) 0.80748(8) 0.00232(12) 0.0304(4) Uani 1 2 d S T P . .
S2 S -0.01968(9) 0.76267(9) -0.14864(9) 0.0270(3) Uani 1 1 d . . . . .
P1 P 0.16029(7) 0.83971(7) 0.13614(11) 0.0241(4) Uani 1 2 d S T P . .
S3 S 0.08831(13) 0.54416(6) 0.08927(13) 0.0269(4) Uani 1 2 d S T P . .
Cs1 Cs 0.333333 0.666667 0.166667 0.176(3) Uani 0.801(9) 12 d S T P . .
Cs2 Cs 0.000000 1.000000 0.000000 0.273(8) Uani 0.707(12) 12 d S T P . .
Cs3 Cs 0.000000 1.000000 -0.228(2) 0.175(13) Uani 0.147(6) 6 d S T P . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

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
Nd1 S2 2.9263(12) . ?
Nd1 S2 2.9263(12) 6 ?
Nd1 S2 2.9486(12) 8_565 ?
Nd1 S2 2.9486(12) 16_454 ?
Nd1 S3 2.9579(10) . ?
Nd1 S3 2.9579(10) 19_565 ?
Nd1 S1 2.9605(4) . ?
Nd1 S1 2.9606(4) 20_455 ?
S1 P1 2.031(2) . ?
S2 P1 2.0268(17) 20_455 ?
S2 Cs3 3.911(9) . ?
P1 S3 2.053(3) 26_455 ?
S3 Cs1 3.6530(18) . ?
Cs1 Cs3 3.69(3) 13_545 ?
Cs1 Cs3 3.69(3) 31_564 ?
Cs2 Cs3 3.08(3) 19_575 ?
Cs2 Cs3 3.08(3) . ?

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
S2 Nd1 S2 87.87(5) . 6 ?
S2 Nd1 S2 136.22(2) . 8_565 ?
S2 Nd1 S2 69.31(4) 6 8_565 ?
S2 Nd1 S2 69.31(4) . 16_454 ?
S2 Nd1 S2 136.22(2) 6 16_454 ?
S2 Nd1 S2 150.33(5) 8_565 16_454 ?
S2 Nd1 S3 154.52(4) . . ?
S2 Nd1 S3 105.05(4) 6 . ?
S2 Nd1 S3 69.25(4) 8_565 . ?
S2 Nd1 S3 86.62(4) 16_454 . ?
S2 Nd1 S3 105.05(4) . 19_565 ?
S2 Nd1 S3 154.52(4) 6 19_565 ?
S2 Nd1 S3 86.62(4) 8_565 19_565 ?
S2 Nd1 S3 69.25(4) 16_454 19_565 ?
S3 Nd1 S3 72.37(5) . 19_565 ?
S2 Nd1 S1 80.20(5) . . ?
S2 Nd1 S1 68.70(4) 6 . ?
S2 Nd1 S1 121.19(4) 8_565 . ?
S2 Nd1 S1 70.84(4) 16_454 . ?
S3 Nd1 S1 84.17(5) . . ?
S3 Nd1 S1 134.37(5) 19_565 . ?
S2 Nd1 S1 68.70(4) . 20_455 ?
S2 Nd1 S1 80.20(5) 6 20_455 ?
S2 Nd1 S1 70.84(4) 8_565 20_455 ?
S2 Nd1 S1 121.19(4) 16_454 20_455 ?
S3 Nd1 S1 134.37(5) . 20_455 ?
S3 Nd1 S1 84.17(5) 19_565 20_455 ?
S1 Nd1 S1 136.52(9) . 20_455 ?
P1 S1 Nd1 86.81(3) . . ?
P1 S1 Nd1 86.81(3) . 21_665 ?
Nd1 S1 Nd1 163.43(9) . 21_665 ?
P1 S2 Nd1 87.82(6) 20_455 . ?
P1 S2 Nd1 90.23(7) 20_455 15_454 ?
Nd1 S2 Nd1 101.61(4) . 15_454 ?
P1 S2 Cs3 101.25(6) 20_455 . ?
Nd1 S2 Cs3 150.6(4) . . ?
Nd1 S2 Cs3 106.2(5) 15_454 . ?
S2 P1 S2 107.31(12) 21_665 6 ?
S2 P1 S1 109.89(7) 21_665 . ?
S2 P1 S1 109.89(7) 6 . ?
S2 P1 S3 110.68(7) 21_665 26_455 ?
S2 P1 S3 110.68(7) 6 26_455 ?
S1 P1 S3 108.38(12) . 26_455 ?
P1 S3 Nd1 89.46(5) 27 19_565 ?
P1 S3 Nd1 89.46(5) 27 . ?
Nd1 S3 Nd1 107.63(5) 19_565 . ?
P1 S3 Cs1 118.02(8) 27 . ?
Nd1 S3 Cs1 121.71(3) 19_565 . ?
Nd1 S3 Cs1 121.71(3) . . ?
S3 Cs1 S3 112.13(3) 2_665 . ?
S3 Cs1 S3 180.0 2_665 26_455 ?
S3 Cs1 S3 67.87(3) . 26_455 ?
S3 Cs1 S3 67.87(3) 2_665 25_565 ?
S3 Cs1 S3 180.0 . 25_565 ?
S3 Cs1 S3 112.13(3) 26_455 25_565 ?
S3 Cs1 S3 67.87(3) 2_665 27 ?
S3 Cs1 S3 67.87(3) . 27 ?
S3 Cs1 S3 112.13(3) 26_455 27 ?
S3 Cs1 S3 112.13(3) 25_565 27 ?
S3 Cs1 S3 112.13(3) 2_665 3_565 ?
S3 Cs1 S3 112.13(3) . 3_565 ?
S3 Cs1 S3 67.87(3) 26_455 3_565 ?
S3 Cs1 S3 67.87(3) 25_565 3_565 ?
S3 Cs1 S3 180.0 27 3_565 ?
S3 Cs1 Cs3 106.66(3) 2_665 13_545 ?
S3 Cs1 Cs3 106.66(3) . 13_545 ?
S3 Cs1 Cs3 73.34(3) 26_455 13_545 ?
S3 Cs1 Cs3 73.34(3) 25_565 13_545 ?
S3 Cs1 Cs3 73.34(3) 27 13_545 ?
S3 Cs1 Cs3 106.66(3) 3_565 13_545 ?
S3 Cs1 Cs3 73.34(3) 2_665 31_564 ?
S3 Cs1 Cs3 73.34(3) . 31_564 ?
S3 Cs1 Cs3 106.66(3) 26_455 31_564 ?
S3 Cs1 Cs3 106.66(3) 25_565 31_564 ?
S3 Cs1 Cs3 106.66(3) 27 31_564 ?
S3 Cs1 Cs3 73.34(3) 3_565 31_564 ?
Cs3 Cs1 Cs3 180.0 13_545 31_564 ?
Cs3 Cs2 Cs3 180.0 19_575 . ?
Cs2 Cs3 Cs1 180.0 . 7_454 ?
Cs2 Cs3 S2 74.2(5) . 2_675 ?
Cs1 Cs3 S2 105.8(5) 7_454 2_675 ?
Cs2 Cs3 S2 74.2(5) . 23_455 ?
Cs1 Cs3 S2 105.8(5) 7_454 23_455 ?
S2 Cs3 S2 147.2(9) 2_675 23_455 ?
Cs2 Cs3 S2 74.2(5) . 22_665 ?
Cs1 Cs3 S2 105.8(5) 7_454 22_665 ?
S2 Cs3 S2 49.34(13) 2_675 22_665 ?
S2 Cs3 S2 112.8(4) 23_455 22_665 ?
Cs2 Cs3 S2 74.2(5) . 24_575 ?
Cs1 Cs3 S2 105.8(5) 7_454 24_575 ?
S2 Cs3 S2 65.63(18) 2_675 24_575 ?
S2 Cs3 S2 112.8(4) 23_455 24_575 ?
S2 Cs3 S2 112.8(4) 22_665 24_575 ?
Cs2 Cs3 S2 74.2(5) . 3_465 ?
Cs1 Cs3 S2 105.8(5) 7_454 3_465 ?
S2 Cs3 S2 112.8(4) 2_675 3_465 ?
S2 Cs3 S2 65.63(17) 23_455 3_465 ?
S2 Cs3 S2 147.2(9) 22_665 3_465 ?
S2 Cs3 S2 49.34(13) 24_575 3_465 ?
Cs2 Cs3 S2 74.2(5) . . ?
Cs1 Cs3 S2 105.8(5) 7_454 . ?
S2 Cs3 S2 112.8(4) 2_675 . ?
S2 Cs3 S2 49.34(13) 23_455 . ?
S2 Cs3 S2 65.63(18) 22_665 . ?
S2 Cs3 S2 147.2(9) 24_575 . ?
S2 Cs3 S2 112.8(4) 3_465 . ?

_refine_diff_density_max         3.258
_refine_diff_density_min         -4.444
_refine_diff_density_rms         0.214


# start Validation Reply Form
_vrf_PLAT974_1                   
;
PROBLEM: Check Calcd Negative Resid. Density on       Cs2      -4.56 eA-3  
RESPONSE: The cesium atoms are severely disordered along the channels in
the structure and cannot be located from the difference map. Due to this
they have been resolved as residing at three positions with overall 
occupancy equal to 0.15 to accomplish charge balance.
;
_vrf_PLAT971_1                   
;
PROBLEM: Check Calcd Resid. Dens.  0.85A   From Cs2             3.20 eA-3  
RESPONSE: The cesium atoms are severely disordered along the channels in
the structure and cannot be located from the difference map. Due to this
they have been resolved as residing at three positions with overall 
occupancy equal to 0.15 to accomplish charge balance.
;
