# Supplementary Information (SI) for Journal of Materials Chemistry C.
# This journal is © The Royal Society of Chemistry 2026

####################################################################### 
# 
# 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_Cu11p95Ni0p05Sb4S13
_database_code_depnum_ccdc_archive 'CCDC 2516851'
loop_
_audit_author_name
_audit_author_address
'Roman Gumeniuk'
;TU Bergakademie Freiberg
Germany
;
_audit_update_record             
;
2025-12-17 deposited with the CCDC.	2026-05-05 downloaded from the CCDC.
;

#------------------  SECTION 2. COMPOUND(S) DETAILS -------------------------#

_audit_creation_date             ?
_audit_creation_method           'WinCSD program'

#------------------ CHEMICAL INFORMATION ------------------------------------#

_chemical_formula_moiety         'Cu11.95 Ni0.05 S13 Sb4'
_chemical_formula_sum            'Cu11.95 Ni0.05 S13 Sb4'
_chemical_formula_weight         1666.31
_chemical_melting_point          ?
_chemical_compound_source        synthetic

loop_
_atom_type_symbol
_atom_type_description
_atom_type_number_in_cell
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
CU Cu 48.00 .125 .419 WinCSD
SB Sb 16.00 -.816 3.315 WinCSD
S S 52.00 .026 .048 WinCSD

#------------------ UNIT CELL INFORMATION -----------------------------------#

loop_
_symmetry_equiv_pos_as_xyz
' x, y, z'
'-y, x, -z'
'-x, -y, z'
' y, -x, -z'
'-x, y, 1/2+z'
' y, x, 1/2-z'
' x, -y, 1/2+z'
'-y, -x, 1/2-z'

_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_H-M   'P -4 c 2'
_symmetry_space_group_name_Hall  'P -4 -2c'

_cell_length_a                   14.5987(4)
_cell_length_b                   14.5987(4)
_cell_length_c                   10.2751(4)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     2189.8(2)
_cell_formula_units_Z            4


#------------------ CRYSTAL INFORMATION -------------------------------------#

_pd_spec_size_axial              ? # mm
_pd_spec_size_equat              0.015 # mm
_pd_spec_size_thick              0.03 # mm


_pd_spec_mounting                
;
packed powder in silica glass capillary
;
_pd_spec_mount_mode              
;
Debye-Scherrer, ID22 beamline-specific
;
_pd_spec_shape                   cylindrical
_pd_char_particle_morphology     ?
_pd_char_colour                  ?

#_pd_prep_conditions               ?
#_pd_prep_cool_rate                ? # K/min
#_pd_prep_pressure                 ? # kPa
#_pd_prep_temperature              ? # K

_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    5.0544
_exptl_crystal_density_method    ?
_exptl_crystal_F_000             3040
_exptl_absorpt_coefficient_mu    7.31

#------------------ DATA COLLECTION INFORMATION -----------------------------#

_cell_measurement_temperature    10
_cell_measurement_reflns_used    4430
_cell_measurement_theta_min      1.00
_cell_measurement_theta_max      20.00

_diffrn_ambient_temperature      10
_diffrn_source_power             ?
_diffrn_source_voltage           ?
_diffrn_source_current           ?
_diffrn_radiation_source         'ESRF, ID22'
_diffrn_measurement_device_type  
;
High-resolution powder diffractometer
;
_diffrn_radiation_detector       2D-detector
_diffrn_radiation_monochromator  Si-111
_diffrn_radiation_probe          'synchrotron X-ray'

_diffrn_radiation_wavelength     0.354600
_diffrn_radiation_type           synchrotron


_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         1.00
_diffrn_reflns_theta_max         20.00


#------------------ COMPUTER PROGRAMS USED ----------------------------------#

_computing_data_collection       ?
_computing_cell_refinement       WinCSD
_computing_data_reduction        WinCSD
_computing_structure_solution    WinCSD
_computing_structure_refinement  WinCSD
_computing_molecular_graphics    ?
_computing_publication_material  'WinCSD (Akselrud et al, 1993)'

#### PLEASE do not forget the following reference :
#L. Akselrud, Yu. Grin.
#WinCSD: software package for crystallographic calculations (Version 4).
#J. Appl. Crystallogr., 2014, 47.

#------------------ REFINEMENT INFORMATION ----------------------------------#

# Use this field to give any special details about
# about the processing of the powder pattern
_pd_proc_ls_special_details      
; ?
;

# The next two items are given as text
_pd_proc_ls_profile_function     pseudo-Voigt
_pd_proc_ls_pref_orient_corr     ?
_pd_proc_ls_prof_R_factor        0.0368
_pd_proc_ls_prof_wR_factor       0.0687
_pd_proc_ls_prof_wR_expected     0.0600
_refine_ls_R_I_factor            0.0489
_refine_ls_goodness_of_fit_all   1.010
_refine_ls_R_factor_all          ?

_refine_special_details          
; ?
;

_refine_ls_structure_factor_coef Inet
_refine_ls_matrix_type           fullcycle

_refine_ls_weighting_scheme      unit
_refine_ls_weighting_details     1/[Yi+σ(Yi)]
_refine_ls_hydrogen_treatment    ?
_refine_ls_extinction_method     ?
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details ?
_refine_ls_abs_structure_Flack   ?
_refine_ls_number_reflns         4430
_refine_ls_number_parameters     59
_refine_ls_number_restraints     ?
_refine_ls_number_constraints    ?
_refine_ls_restrained_S_all      ?
_refine_ls_restrained_S_obs      ?
_refine_ls_shift/su_max          ?
_refine_ls_shift/su_mean         ?

_refine_diff_density_max         3.38
_refine_diff_density_min         -2.52

#------------------ ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS --------#

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_thermal_displace_type
_atom_site_B_iso_or_equiv
_atom_site_symmetry_multiplicity
_atom_site_occupancy
Cu1 CU 0.5 0.5 0 Biso 0.44(8) 2 1.0
Cu2 CU 0 0 0 Biso 0.46(7) 2 1.0
Cu3 CU 0.1375(6) 0.13758 0.75 Biso 0.39(5) 4 1.0
Cu4 CU 0.3808(6) 0.38083 0.75 Biso 0.25(5) 4 1.0
Cu5 CU 0 0.5 0.027(1) Biso 0.63(6) 4 1.0
Cu6 CU 0.3524(6) 0.35248 0.25 Biso 1.82(6) 4 1.0
Cu7 CU 0.1262(6) 0.12628 0.25 Biso 0.97(5) 4 1.0
Cu8 CU 0.6257(7) 0.1223(6) 0.2402(9) Biso 0.61(4) 8 1.0
Cu9 CU 0.3612(5) 0.1512(6) 0.2178(7) Biso 1.02(4) 8 1.0
Cu10 CU 0.2720(5) 0.2509(6) 0.0416(6) Biso 0.93(4) 8 1.0
Sb1 SB 0.2536(4) 0.4775(2) 0.0234(4) Biso 0.70(2) 8 1.0
Sb2 SB 0.2556(4) 0.0073(2) 0.0082(4) Biso 0.76(2) 8 1.0
S1 S 0.2329(8) 0.23293 0.25 Biso 1.08(9) 4 1.0
S2 S 0.250(2) 0.147(1) 0.597(1) Biso 0.45(7) 8 1.0
S3 S 0.250(2) 0.628(1) 0.122(2) Biso 0.44(6) 8 1.0
S4 S 0.016(1) 0.372(2) 0.153(2) Biso 0.55(9) 8 1.0
S5 S 0.000(1) 0.122(2) 0.138(2) Biso 0.82(9) 8 1.0
S6 S 0.484(1) 0.372(2) 0.133(2) Biso 0.39(7) 8 1.0
S7 S 0.493(1) 0.124(2) 0.118(2) Biso 0.52(8) 8 1.0


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
Cu1 S6 2.33(2) . yes
Cu1 Cu4 3.557(6) 1_554 yes
Cu1 Sb1 3.620(6) . yes
Cu2 S5 2.29(2) . yes
Cu2 Sb2 3.735(6) . yes
Cu3 S2 2.28(2) . yes
Cu3 S5 2.34(2) 4_556 yes
Cu3 Cu8 3.464(12) 4_566 yes
Cu3 Sb2 3.690(7) 2_556 yes
Cu3 Sb2 3.692(7) 1_556 yes
Cu4 S6 2.30(2) 4_566 yes
Cu4 S3 2.31(2) 2_656 yes
Cu4 Sb1 3.625(8) 2_656 yes
Cu4 Sb1 3.652(7) 1_556 yes
Cu5 S4 2.28(2) . yes
Cu5 S7 2.36(2) 2_555 yes
Cu5 Cu8 3.501(13) 6_555 yes
Cu5 Sb2 3.588(6) 2_555 yes
Cu5 Sb1 3.717(6) . yes
Cu6 S6 2.29(2) . yes
Cu6 S1 2.468(14) . yes
Cu6 Cu10 2.856(9) . yes
Cu6 Cu9 2.960(12) . yes
Cu6 Sb1 3.292(8) . yes
Cu7 S5 2.16(2) . yes
Cu7 S1 2.202(14) . yes
Cu7 Cu9 3.465(11) . yes
Cu7 Cu10 3.525(10) . yes
Cu7 Sb2 3.571(7) . yes
Cu7 Sb2 3.797(7) 2_555 yes
Cu8 S7 2.29(2) . yes
Cu8 S4 2.30(2) 8_655 yes
Cu8 S3 2.34(2) 6_555 yes
Cu8 S2 2.36(2) 5_654 yes
Cu8 Sb2 3.502(10) 3_655 yes
Cu8 Sb1 3.646(10) 2_655 yes
Cu8 Sb2 3.661(10) 5_655 yes
Cu8 Sb1 3.774(10) 6_555 yes
Cu9 S7 2.22(2) . yes
Cu9 S1 2.246(13) . yes
Cu9 S4 2.38(2) 6_555 yes
Cu9 Cu10 2.663(10) . yes
Cu9 Sb2 3.380(9) . yes
Cu9 Cu10 3.437(10) 6_555 yes
Cu9 Sb1 3.491(9) 6_555 yes
Cu9 Sb1 3.731(9) 2_655 yes
Cu10 S1 2.231(7) . yes
Cu10 S3 2.23(2) 2_655 yes
Cu10 S2 2.31(2) 6_555 yes
Cu10 Sb1 3.324(9) . yes
Cu10 Sb2 3.581(9) . yes
Cu10 Sb1 3.716(7) 2_655 yes
Sb1 S7 2.42(2) 4_565 yes
Sb1 S6 2.42(2) 4_565 yes
Sb1 S3 2.43(2) . yes
Sb1 S2 3.86(2) 6_555 yes
Sb1 S6 3.88(2) . yes
Sb1 S6 3.93(2) 6_555 yes
Sb2 S4 2.40(2) 4_555 yes
Sb2 S2 2.445(15) 7_554 yes
Sb2 S5 2.46(2) 4_555 yes
Sb2 S4 3.87(2) 6_555 yes
S2 S3 3.28(2) 7_565 yes
S2 S4 3.67(2) 6_555 yes
S2 S3 3.69(2) 2_656 yes
S3 S7 3.57(3) 4_565 yes
S3 S6 3.58(3) 4_565 yes
S3 S3 3.62(2) 8_665 yes
S4 S7 3.34(3) 6_555 yes
S4 S5 3.65(3) . yes
S4 S7 3.68(3) 8_565 yes
S5 S5 3.41(3) 6_555 yes
S5 S5 3.44(3) 8_555 yes
S5 S5 3.59(3) 3_555 yes
S6 S6 3.35(3) 6_555 yes
S6 S7 3.62(3) . yes
S7 S7 3.64(3) 3_655 yes

# start Validation Reply Form
_vrf_GEOM006_Cu11.95Ni0.05Sb4S13 
;
PROBLEM: _geom_angle_atom_site_label_2 is missing
RESPONSE: "inorganic structure"
;
_vrf_GEOM007_Cu11.95Ni0.05Sb4S13 
;
PROBLEM: _geom_angle_atom_site_label_3 is missing
RESPONSE: "inorganic structure"
;
_vrf_GEOM008_Cu11.95Ni0.05Sb4S13 
;
PROBLEM: _geom_angle is missing
RESPONSE: "inorganic structure"
;
_vrf_WEIGH01_Cu11.95Ni0.05Sb4S13 
;
PROBLEM: Unit weights are not acceptable for submissions to Acta
RESPONSE: "not Acta-journal submission"
;
####################################################################### 
# 
# 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_Cu11p95Ni0p05Sb4S13_CCDC1
_database_code_depnum_ccdc_archive 'CCDC 2516849'
loop_
_audit_author_name
_audit_author_address
'Roman Gumeniuk'
;TU Bergakademie Freiberg
Germany
;
_audit_update_record             
;
2025-12-17 deposited with the CCDC.	2026-05-05 downloaded from the CCDC.
;

#------------------  SECTION 2. COMPOUND(S) DETAILS -------------------------#

_audit_creation_date             ?
_audit_creation_method           'WinCSD program'

#------------------ CHEMICAL INFORMATION ------------------------------------#

_chemical_formula_moiety         'Cu11.95 Ni0.05 S13 Sb4'
_chemical_formula_sum            'Cu11.95 Ni0.05 S13 Sb4'
_chemical_formula_weight         1666.31
_chemical_melting_point          ?
_chemical_compound_source        synthetic

loop_
_atom_type_symbol
_atom_type_description
_atom_type_number_in_cell
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
CU Cu 24.00 .125 .419 WinCSD
SB Sb 8.00 -.816 3.315 WinCSD
S S 26.00 .026 .048 WinCSD

#------------------ UNIT CELL INFORMATION -----------------------------------#

loop_
_symmetry_equiv_pos_as_xyz
' x, y, z'
' z, x, y'
' y, z, x'
'-y, x, -z'
'-x, z, -y'
'-z, y, -x'
' x, -y, -z'
' z, -x, -y'
' y, -z, -x'
'-y, -x, z'
'-x, -z, y'
'-z, -y, x'
'-x, y, -z'
'-z, x, -y'
'-y, z, -x'
' y, x, z'
' x, z, y'
' z, y, x'
'-x, -y, z'
'-z, -x, y'
'-y, -z, x'
' y, -x, -z'
' x, -z, -y'
' z, -y, -x'
' 1/2+x, 1/2+y, 1/2+z'
' 1/2+z, 1/2+x, 1/2+y'
' 1/2+y, 1/2+z, 1/2+x'
' 1/2-y, 1/2+x, 1/2-z'
' 1/2-x, 1/2+z, 1/2-y'
' 1/2-z, 1/2+y, 1/2-x'
' 1/2+x, 1/2-y, 1/2-z'
' 1/2+z, 1/2-x, 1/2-y'
' 1/2+y, 1/2-z, 1/2-x'
' 1/2-y, 1/2-x, 1/2+z'
' 1/2-x, 1/2-z, 1/2+y'
' 1/2-z, 1/2-y, 1/2+x'
' 1/2-x, 1/2+y, 1/2-z'
' 1/2-z, 1/2+x, 1/2-y'
' 1/2-y, 1/2+z, 1/2-x'
' 1/2+y, 1/2+x, 1/2+z'
' 1/2+x, 1/2+z, 1/2+y'
' 1/2+z, 1/2+y, 1/2+x'
' 1/2-x, 1/2-y, 1/2+z'
' 1/2-z, 1/2-x, 1/2+y'
' 1/2-y, 1/2-z, 1/2+x'
' 1/2+y, 1/2-x, 1/2-z'
' 1/2+x, 1/2-z, 1/2-y'
' 1/2+z, 1/2-y, 1/2-x'

_symmetry_cell_setting           cubic
_symmetry_space_group_name_H-M   'I -4 3 m'
_symmetry_space_group_name_Hall  'I -4 2 3'

_cell_length_a                   10.33768(3)
_cell_length_b                   10.33768(3)
_cell_length_c                   10.33768(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1104.76(1)
_cell_formula_units_Z            2

#------------------ CRYSTAL INFORMATION -------------------------------------#

_pd_spec_size_axial              ? # mm
_pd_spec_size_equat              0.015 # mm
_pd_spec_size_thick              0.03 # mm

_pd_spec_mounting                
;
packed powder in silica glass capillary
;
_pd_spec_mount_mode              
;
Debye-Scherrer, ID22 beamline-specific
;
_pd_spec_shape                   cylindrical
_pd_char_particle_morphology     ?
_pd_char_colour                  ?

#_pd_prep_conditions               ?
#_pd_prep_cool_rate                ? # K/min
#_pd_prep_pressure                 ? # kPa
#_pd_prep_temperature              ? # K

_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    5.0094
_exptl_crystal_density_method    ?
_exptl_crystal_F_000             1520
_exptl_absorpt_coefficient_mu    7.25

#------------------ DATA COLLECTION INFORMATION -----------------------------#

_cell_measurement_temperature    293
_cell_measurement_reflns_used    443
_cell_measurement_theta_min      1.00
_cell_measurement_theta_max      20.00

_diffrn_ambient_temperature      293
_diffrn_source_power             ?
_diffrn_source_voltage           ?
_diffrn_source_current           ?
_diffrn_radiation_source         'ESRF, ID22'
_diffrn_measurement_device_type  
;
High-resolution powder diffractometer
;
_diffrn_radiation_detector       2D-detector
_diffrn_radiation_monochromator  Si-111
_diffrn_radiation_probe          'synchrotron X-ray'

_diffrn_radiation_wavelength     0.354600
_diffrn_radiation_type           synchrotron

_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       1
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         1.00
_diffrn_reflns_theta_max         20.00


#------------------ COMPUTER PROGRAMS USED ----------------------------------#

_computing_data_collection       ?
_computing_cell_refinement       WinCSD
_computing_data_reduction        WinCSD
_computing_structure_solution    WinCSD
_computing_structure_refinement  WinCSD
_computing_molecular_graphics    ?
_computing_publication_material  'WinCSD (Akselrud et al, 1993)'

#### PLEASE do not forget the following reference :
#L. Akselrud, Yu. Grin.
#WinCSD: software package for crystallographic calculations (Version 4).
#J. Appl. Crystallogr., 2014, 47.

#------------------ REFINEMENT INFORMATION ----------------------------------#

# Use this field to give any special details about
# about the processing of the powder pattern
_pd_proc_ls_special_details      
; ?
;

# The next two items are given as text
_pd_proc_ls_profile_function     pseudo-Voigt
_pd_proc_ls_pref_orient_corr     ?
_pd_proc_ls_prof_R_factor        0.0285
_pd_proc_ls_prof_wR_factor       0.0468
_pd_proc_ls_prof_wR_expected     0.0765
_refine_ls_R_I_factor            0.0398
_refine_ls_goodness_of_fit_all   1.010
_refine_ls_R_factor_all          ?

_refine_special_details          
; ?
;

_refine_ls_structure_factor_coef Inet
_refine_ls_matrix_type           fullcycle

_refine_ls_weighting_scheme      unit
_refine_ls_weighting_details     1/[Yi+σ(Yi)]
_refine_ls_hydrogen_treatment    ?
_refine_ls_extinction_method     ?
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details ?
_refine_ls_abs_structure_Flack   ?
_refine_ls_number_reflns         443
_refine_ls_number_parameters     11
_refine_ls_number_restraints     ?
_refine_ls_number_constraints    ?
_refine_ls_restrained_S_all      ?
_refine_ls_restrained_S_obs      ?
_refine_ls_shift/su_max          ?
_refine_ls_shift/su_mean         ?

_refine_diff_density_max         1.82
_refine_diff_density_min         -1.50

#------------------ ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS --------#

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_thermal_displace_type
_atom_site_B_iso_or_equiv
_atom_site_symmetry_multiplicity
_atom_site_occupancy
Cu1 CU 0.25 0.5 0 Biso 1.91(1) 12 1.0
Cu2 CU 0.02067(6) 0.02067 0.78305(5) Biso 2.89(2) 24 0.5
Sb1 SB 0.26816(2) 0.26816 0.26816 Biso 1.472(4) 8 1.0
S1 S 0 0 0 Biso 1.73(5) 2 1.0
S2 S 0.11507(5) 0.11507 0.36216(6) Biso 1.30(1) 24 1.0


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
Cu1 S2 2.3218(6) 3_555 yes
Cu1 Sb1 3.6694(2) . yes
Cu2 Cu2 0.6045(8) 10_555 yes
Cu2 S1 2.2630(6) 1_556 yes
Cu2 S2 2.2750(8) 4_556 yes
Cu2 Cu2 2.8693(8) 6_656 yes
Cu2 Sb1 3.0909(6) 34_555 yes
Cu2 Cu2 3.2145(8) 5_546 yes
Cu2 Cu2 3.4739(8) 2_456 yes
Cu2 Sb1 3.6949(6) 25_445 yes
Sb1 S2 2.4399(6) . yes
S2 S2 3.3648(7) 10_555 yes
S2 S2 3.6124(8) 2_555 yes

# start Validation Reply Form
_vrf_GEOM006_Cu11.95Ni0.05Sb4S13 
;
PROBLEM: _geom_angle_atom_site_label_2 is missing
RESPONSE: "inorganic structure"
;
_vrf_GEOM007_Cu11.95Ni0.05Sb4S13 
;
PROBLEM: _geom_angle_atom_site_label_3 is missing
RESPONSE: "inorganic structure"
;
_vrf_GEOM008_Cu11.95Ni0.05Sb4S13 
;
PROBLEM: _geom_angle is missing
RESPONSE: "inorganic structure"
;
_vrf_WEIGH01_Cu11.95Ni0.05Sb4S13 
;
PROBLEM: Unit weights are not acceptable for submissions to Acta
RESPONSE: "not Acta-journal submission"
;
####################################################################### 
# 
# 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_Cu12S13Sb4
_database_code_depnum_ccdc_archive 'CCDC 2516853'
loop_
_audit_author_name
_audit_author_address
'Roman Gumeniuk'
;TU Bergakademie Freiberg
Germany
;
_audit_update_record             
;
2025-12-17 deposited with the CCDC.	2026-05-05 downloaded from the CCDC.
;

#------------------  SECTION 2. COMPOUND(S) DETAILS -------------------------#

_audit_creation_date             ?
_audit_creation_method           'WinCSD program'

#------------------ CHEMICAL INFORMATION ------------------------------------#
_chemical_formula_moiety         'Cu12 S13 Sb4'
_chemical_formula_sum            'Cu12 S13 Sb4'
_chemical_formula_weight         1666.55
_chemical_melting_point          ?
_chemical_compound_source        synthetic

loop_
_atom_type_symbol
_atom_type_description
_atom_type_number_in_cell
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
CU Cu 24.00 .125 .419 WinCSD
SB Sb 8.00 -.816 3.315 WinCSD
S S 26.00 .026 .048 WinCSD

#------------------ UNIT CELL INFORMATION -----------------------------------#

loop_
_symmetry_equiv_pos_as_xyz
' x, y, z'
' z, x, y'
' y, z, x'
'-y, x, -z'
'-x, z, -y'
'-z, y, -x'
' x, -y, -z'
' z, -x, -y'
' y, -z, -x'
'-y, -x, z'
'-x, -z, y'
'-z, -y, x'
'-x, y, -z'
'-z, x, -y'
'-y, z, -x'
' y, x, z'
' x, z, y'
' z, y, x'
'-x, -y, z'
'-z, -x, y'
'-y, -z, x'
' y, -x, -z'
' x, -z, -y'
' z, -y, -x'
' 1/2+x, 1/2+y, 1/2+z'
' 1/2+z, 1/2+x, 1/2+y'
' 1/2+y, 1/2+z, 1/2+x'
' 1/2-y, 1/2+x, 1/2-z'
' 1/2-x, 1/2+z, 1/2-y'
' 1/2-z, 1/2+y, 1/2-x'
' 1/2+x, 1/2-y, 1/2-z'
' 1/2+z, 1/2-x, 1/2-y'
' 1/2+y, 1/2-z, 1/2-x'
' 1/2-y, 1/2-x, 1/2+z'
' 1/2-x, 1/2-z, 1/2+y'
' 1/2-z, 1/2-y, 1/2+x'
' 1/2-x, 1/2+y, 1/2-z'
' 1/2-z, 1/2+x, 1/2-y'
' 1/2-y, 1/2+z, 1/2-x'
' 1/2+y, 1/2+x, 1/2+z'
' 1/2+x, 1/2+z, 1/2+y'
' 1/2+z, 1/2+y, 1/2+x'
' 1/2-x, 1/2-y, 1/2+z'
' 1/2-z, 1/2-x, 1/2+y'
' 1/2-y, 1/2-z, 1/2+x'
' 1/2+y, 1/2-x, 1/2-z'
' 1/2+x, 1/2-z, 1/2-y'
' 1/2+z, 1/2-y, 1/2-x'

_symmetry_cell_setting           cubic
_symmetry_space_group_name_H-M   'I -4 3 m'
_symmetry_space_group_name_Hall  'I -4 2 3'

_cell_length_a                   10.32352(3)
_cell_length_b                   10.32352(3)
_cell_length_c                   10.32352(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1100.231(9)
_cell_formula_units_Z            2

#------------------ CRYSTAL INFORMATION -------------------------------------#

_pd_spec_size_axial              ? # mm
_pd_spec_size_equat              0.015 # mm
_pd_spec_size_thick              0.03 # mm

_pd_spec_mounting                
;
packed powder in silica glass capillary
;
_pd_spec_mount_mode              
;
Debye-Scherrer, ID22 beamline-specific
;
_pd_spec_shape                   cylindrical
_pd_char_particle_morphology     ?
_pd_char_colour                  ?

#_pd_prep_conditions               ?
#_pd_prep_cool_rate                ? # K/min
#_pd_prep_pressure                 ? # kPa
#_pd_prep_temperature              ? # K

_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    5.0301
_exptl_crystal_density_method    ?
_exptl_crystal_F_000             1520
_exptl_absorpt_coefficient_mu    7.28

#------------------ DATA COLLECTION INFORMATION -----------------------------#

_cell_measurement_temperature    293
_cell_measurement_reflns_used    443
_cell_measurement_theta_min      1.00
_cell_measurement_theta_max      20.00

_diffrn_ambient_temperature      293
_diffrn_source_power             ?
_diffrn_source_voltage           ?
_diffrn_source_current           ?
_diffrn_radiation_source         'ESRF, ID22'
_diffrn_measurement_device_type  
;
High-resolution powder diffractometer
;
_diffrn_radiation_detector       2D-detector
_diffrn_radiation_monochromator  Si-111
_diffrn_radiation_probe          'synchrotron X-ray'

_diffrn_radiation_wavelength     0.354600
_diffrn_radiation_type           synchrotron

_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       1
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         1.00
_diffrn_reflns_theta_max         20.00

#------------------ COMPUTER PROGRAMS USED ----------------------------------#

_computing_data_collection       ?
_computing_cell_refinement       WinCSD
_computing_data_reduction        WinCSD
_computing_structure_solution    WinCSD
_computing_structure_refinement  WinCSD
_computing_molecular_graphics    ?
_computing_publication_material  'WinCSD (Akselrud et al, 1993)'

#### PLEASE do not forget the following reference :
#L. Akselrud, Yu. Grin.
#WinCSD: software package for crystallographic calculations (Version 4).
#J. Appl. Crystallogr., 2014, 47.

#------------------ REFINEMENT INFORMATION ----------------------------------#

# Use this field to give any special details about
# about the processing of the powder pattern
_pd_proc_ls_special_details      
; ?
;

# The next two items are given as text
_pd_proc_ls_profile_function     pseudo-Voigt
_pd_proc_ls_pref_orient_corr     ?
_pd_proc_ls_prof_R_factor        0.0294
_pd_proc_ls_prof_wR_factor       0.0404
_pd_proc_ls_prof_wR_expected     0.0564
_refine_ls_R_I_factor            0.0449
_refine_ls_goodness_of_fit_all   1.010
_refine_ls_R_factor_all          ?

_refine_special_details          
; ?
;

_refine_ls_structure_factor_coef Inet
_refine_ls_matrix_type           fullcycle

_refine_ls_weighting_scheme      unit
_refine_ls_weighting_details     1/[Yi+σ(Yi)]
_refine_ls_hydrogen_treatment    ?
_refine_ls_extinction_method     ?
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details ?
_refine_ls_abs_structure_Flack   ?
_refine_ls_number_reflns         443
_refine_ls_number_parameters     11
_refine_ls_number_restraints     ?
_refine_ls_number_constraints    ?
_refine_ls_restrained_S_all      ?
_refine_ls_restrained_S_obs      ?
_refine_ls_shift/su_max          ?
_refine_ls_shift/su_mean         ?

_refine_diff_density_max         1.19
_refine_diff_density_min         -0.88

#------------------ ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS --------#

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_thermal_displace_type
_atom_site_B_iso_or_equiv
_atom_site_symmetry_multiplicity
_atom_site_occupancy
Cu1 Cu 0.25 0.5 0 Biso 1.65(1) 12 1.0
Cu2 Cu 0.02036(5) 0.02036 0.78162(5) Biso 2.40(2) 24 0.5
Sb1 Sb 0.26859(2) 0.26859 0.26859 Biso 1.279(4) 8 1.0
S1 S 0 0 0 Biso 1.66(5) 2 1.0
S2 S 0.11536(5) 0.11536 0.36387(6) Biso 1.00(1) 24 1.0

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
Cu1 S2 2.3076(5) 3_555 yes
Cu1 Sb1 3.6650(2) . yes
Cu2 Cu2 0.5946(8) 10_555 yes
Cu2 S1 2.2739(6) 1_556 yes
Cu2 S2 2.2763(8) 4_556 yes
Cu2 Cu2 2.8909(8) 6_656 yes
Cu2 Sb1 3.0841(6) 34_555 yes
Cu2 Cu2 3.2295(8) 5_546 yes
Cu2 Cu2 3.4855(8) 2_456 yes
Cu2 Sb1 3.6782(6) 25_445 yes
Sb1 S2 2.4438(5) . yes
S2 S2 3.3686(7) 10_555 yes
S2 S2 3.6282(8) 2_555 yes
S2 S2 3.6842(8) 4_556 yes

# start Validation Reply Form
_vrf_GEOM006_Cu12S13Sb4          
;
PROBLEM: _geom_angle_atom_site_label_2 is missing
RESPONSE: "inorganic structure"
;
_vrf_GEOM007_Cu12S13Sb4          
;
PROBLEM: _geom_angle_atom_site_label_3 is missing
RESPONSE: "inorganic structure"
;
_vrf_GEOM008_Cu12S13Sb4          
;
PROBLEM: _geom_angle is missing
RESPONSE: "inorganic structure"
;
_vrf_WEIGH01_Cu12S13Sb4          
;
PROBLEM: Unit weights are not acceptable for submissions to Acta
RESPONSE: "not Acta-journal submission"
;
####################################################################### 
# 
# 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_Cu11p8Ni0p2Sb4S13
_database_code_depnum_ccdc_archive 'CCDC 2516847'
loop_
_audit_author_name
_audit_author_address
'Roman Gumeniuk'
;TU Bergakademie Freiberg
Germany
;
_audit_update_record             
;
2025-12-17 deposited with the CCDC.	2026-05-05 downloaded from the CCDC.
;

#------------------  SECTION 2. COMPOUND(S) DETAILS -------------------------#

_audit_creation_date             ?
_audit_creation_method           'WinCSD program'

#------------------ CHEMICAL INFORMATION ------------------------------------#

_chemical_formula_moiety         'Cu11.8 Ni0.2 S13 Sb4'
_chemical_formula_sum            'Cu11.8 Ni0.2 S13 Sb4'
_chemical_formula_weight         1665.62
_chemical_melting_point          ?
_chemical_compound_source        synthetic

loop_
_atom_type_symbol
_atom_type_description
_atom_type_number_in_cell
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
CU Cu 24.00 .125 .419 WinCSD
SB Sb 8.00 -.816 3.315 WinCSD
S S 26.00 .026 .048 WinCSD

#------------------ UNIT CELL INFORMATION -----------------------------------#

loop_
_symmetry_equiv_pos_as_xyz
' x, y, z'
' z, x, y'
' y, z, x'
'-y, x, -z'
'-x, z, -y'
'-z, y, -x'
' x, -y, -z'
' z, -x, -y'
' y, -z, -x'
'-y, -x, z'
'-x, -z, y'
'-z, -y, x'
'-x, y, -z'
'-z, x, -y'
'-y, z, -x'
' y, x, z'
' x, z, y'
' z, y, x'
'-x, -y, z'
'-z, -x, y'
'-y, -z, x'
' y, -x, -z'
' x, -z, -y'
' z, -y, -x'
' 1/2+x, 1/2+y, 1/2+z'
' 1/2+z, 1/2+x, 1/2+y'
' 1/2+y, 1/2+z, 1/2+x'
' 1/2-y, 1/2+x, 1/2-z'
' 1/2-x, 1/2+z, 1/2-y'
' 1/2-z, 1/2+y, 1/2-x'
' 1/2+x, 1/2-y, 1/2-z'
' 1/2+z, 1/2-x, 1/2-y'
' 1/2+y, 1/2-z, 1/2-x'
' 1/2-y, 1/2-x, 1/2+z'
' 1/2-x, 1/2-z, 1/2+y'
' 1/2-z, 1/2-y, 1/2+x'
' 1/2-x, 1/2+y, 1/2-z'
' 1/2-z, 1/2+x, 1/2-y'
' 1/2-y, 1/2+z, 1/2-x'
' 1/2+y, 1/2+x, 1/2+z'
' 1/2+x, 1/2+z, 1/2+y'
' 1/2+z, 1/2+y, 1/2+x'
' 1/2-x, 1/2-y, 1/2+z'
' 1/2-z, 1/2-x, 1/2+y'
' 1/2-y, 1/2-z, 1/2+x'
' 1/2+y, 1/2-x, 1/2-z'
' 1/2+x, 1/2-z, 1/2-y'
' 1/2+z, 1/2-y, 1/2-x'

_symmetry_cell_setting           cubic
_symmetry_space_group_name_H-M   'I -4 3 m'
_symmetry_space_group_name_Hall  'I -4 2 3'

_cell_length_a                   10.32964(2)
_cell_length_b                   10.32964(2)
_cell_length_c                   10.32964(2)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1102.189(6)
_cell_formula_units_Z            2


#------------------ CRYSTAL INFORMATION -------------------------------------#

_pd_spec_size_axial              ? # mm
_pd_spec_size_equat              0.015 # mm
_pd_spec_size_thick              0.03 # mm

_pd_spec_mounting                
;
packed powder in silica glass capillary
;
_pd_spec_mount_mode              
;
Debye-Scherrer, ID22 beamline-specific
;
_pd_spec_shape                   cylindrical
_pd_char_particle_morphology     ?
_pd_char_colour                  ?

#_pd_prep_conditions               ?
#_pd_prep_cool_rate                ? # K/min
#_pd_prep_pressure                 ? # kPa
#_pd_prep_temperature              ? # K

_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    5.0211
_exptl_crystal_density_method    ?
_exptl_crystal_F_000             1520
_exptl_absorpt_coefficient_mu    7.27

#------------------ DATA COLLECTION INFORMATION -----------------------------#

_cell_measurement_temperature    293
_cell_measurement_reflns_used    443
_cell_measurement_theta_min      1.00
_cell_measurement_theta_max      20.00

_diffrn_ambient_temperature      293
_diffrn_source_power             ?
_diffrn_source_voltage           ?
_diffrn_source_current           ?
_diffrn_radiation_source         'ESRF, ID22'
_diffrn_measurement_device_type  
;
High-resolution powder diffractometer
;
_diffrn_radiation_detector       2D-detector
_diffrn_radiation_monochromator  Si-111
_diffrn_radiation_probe          'synchrotron X-ray'

_diffrn_radiation_wavelength     0.354600
_diffrn_radiation_type           synchrotron

_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       1
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         1.00
_diffrn_reflns_theta_max         20.00


#------------------ COMPUTER PROGRAMS USED ----------------------------------#

_computing_data_collection       ?
_computing_cell_refinement       WinCSD
_computing_data_reduction        WinCSD
_computing_structure_solution    WinCSD
_computing_structure_refinement  WinCSD
_computing_molecular_graphics    ?
_computing_publication_material  'WinCSD (Akselrud et al, 1993)'

#### PLEASE do not forget the following reference :
#L. Akselrud, Yu. Grin.
#WinCSD: software package for crystallographic calculations (Version 4).
#J. Appl. Crystallogr., 2014, 47.

#------------------ REFINEMENT INFORMATION ----------------------------------#

# Use this field to give any special details about
# about the processing of the powder pattern
_pd_proc_ls_special_details      
; ?
;

# The next two items are given as text
_pd_proc_ls_profile_function     pseudo-Voigt
_pd_proc_ls_pref_orient_corr     ?
_pd_proc_ls_prof_R_factor        0.0254
_pd_proc_ls_prof_wR_factor       0.0386
_pd_proc_ls_prof_wR_expected     0.0762
_refine_ls_R_I_factor            0.0323
_refine_ls_goodness_of_fit_all   1.010
_refine_ls_R_factor_all          ?

_refine_special_details          
; ?
;

_refine_ls_structure_factor_coef Inet
_refine_ls_matrix_type           fullcycle

_refine_ls_weighting_scheme      unit
_refine_ls_weighting_details     1/[Yi+σ(Yi)]
_refine_ls_hydrogen_treatment    ?
_refine_ls_extinction_method     ?
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details ?
_refine_ls_abs_structure_Flack   ?
_refine_ls_number_reflns         443
_refine_ls_number_parameters     11
_refine_ls_number_restraints     ?
_refine_ls_number_constraints    ?
_refine_ls_restrained_S_all      ?
_refine_ls_restrained_S_obs      ?
_refine_ls_shift/su_max          ?
_refine_ls_shift/su_mean         ?

_refine_diff_density_max         1.19
_refine_diff_density_min         -0.88

#------------------ ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS --------#

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_thermal_displace_type
_atom_site_B_iso_or_equiv
_atom_site_symmetry_multiplicity
_atom_site_occupancy
Cu1 CU 0.25 0.5 0 Biso 1.731(8) 12 1.0
Cu2 CU 0.02032(4) 0.02032 0.78272(4) Biso 2.66(2) 24 0.5
Sb1 SB 0.26841(1) 0.26841 0.26841 Biso 1.308(3) 8 1.0
S1 S 0 0 0 Biso 1.92(4) 2 1.0
S2 S 0.11535(4) 0.11535 0.36253(5) Biso 1.178(8) 24 1.0


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
Cu1 S2 2.3174(4) 3_555 yes
Cu1 Sb1 3.6669(2) . yes
Cu2 Cu2 0.5938(6) 10_555 yes
Cu2 S1 2.2640(5) 1_556 yes
Cu2 S2 2.2758(6) 4_556 yes
Cu2 Cu2 2.8772(6) 6_656 yes
Cu2 Sb1 3.0897(5) 34_555 yes
Cu2 Cu2 3.2155(6) 5_546 yes
Cu2 Cu2 3.4710(6) 2_456 yes
Cu2 Sb1 3.6829(5) 25_445 yes
Sb1 S2 2.4382(4) . yes
S2 S2 3.3704(5) 10_555 yes
S2 S2 3.6109(6) 2_555 yes

# start Validation Reply Form
_vrf_GEOM006_Cu11.8Ni0.2Sb4S13   
;
PROBLEM: _geom_angle_atom_site_label_2 is missing
RESPONSE: "inorganic structure"
;
_vrf_GEOM007_Cu11.8Ni0.2Sb4S13   
;
PROBLEM: _geom_angle_atom_site_label_3 is missing
RESPONSE: "inorganic structure"
;
_vrf_GEOM008_Cu11.8Ni0.2Sb4S13   
;
PROBLEM: _geom_angle is missing
RESPONSE: "inorganic structure"
;
_vrf_WEIGH01_Cu11.8Ni0.2Sb4S13   
;
PROBLEM: Unit weights are not acceptable for submissions to Acta
RESPONSE: "not Acta-journal submission"
;
####################################################################### 
# 
# 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_Cu11p5Ni0p5Sb4S13
_database_code_depnum_ccdc_archive 'CCDC 2516852'
loop_
_audit_author_name
_audit_author_address
'Roman Gumeniuk'
;TU Bergakademie Freiberg
Germany
;
_audit_update_record             
;
2025-12-17 deposited with the CCDC.	2026-05-05 downloaded from the CCDC.
;

#------------------  SECTION 2. COMPOUND(S) DETAILS -------------------------#

_audit_creation_date             ?
_audit_creation_method           'WinCSD program'

#------------------ CHEMICAL INFORMATION ------------------------------------#

_chemical_formula_moiety         'Cu11.5 Ni0.5 S13 Sb4'
_chemical_formula_sum            'Cu11.5 Ni0.5 S13 Sb4'
_chemical_formula_weight         1664.12
_chemical_melting_point          ?
_chemical_compound_source        synthetic

loop_
_atom_type_symbol
_atom_type_description
_atom_type_number_in_cell
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
CU Cu 24.00 .125 .419 WinCSD
SB Sb 8.00 -.816 3.315 WinCSD
S S 26.00 .026 .048 WinCSD

#------------------ UNIT CELL INFORMATION -----------------------------------#

loop_
_symmetry_equiv_pos_as_xyz
' x, y, z'
' z, x, y'
' y, z, x'
'-y, x, -z'
'-x, z, -y'
'-z, y, -x'
' x, -y, -z'
' z, -x, -y'
' y, -z, -x'
'-y, -x, z'
'-x, -z, y'
'-z, -y, x'
'-x, y, -z'
'-z, x, -y'
'-y, z, -x'
' y, x, z'
' x, z, y'
' z, y, x'
'-x, -y, z'
'-z, -x, y'
'-y, -z, x'
' y, -x, -z'
' x, -z, -y'
' z, -y, -x'
' 1/2+x, 1/2+y, 1/2+z'
' 1/2+z, 1/2+x, 1/2+y'
' 1/2+y, 1/2+z, 1/2+x'
' 1/2-y, 1/2+x, 1/2-z'
' 1/2-x, 1/2+z, 1/2-y'
' 1/2-z, 1/2+y, 1/2-x'
' 1/2+x, 1/2-y, 1/2-z'
' 1/2+z, 1/2-x, 1/2-y'
' 1/2+y, 1/2-z, 1/2-x'
' 1/2-y, 1/2-x, 1/2+z'
' 1/2-x, 1/2-z, 1/2+y'
' 1/2-z, 1/2-y, 1/2+x'
' 1/2-x, 1/2+y, 1/2-z'
' 1/2-z, 1/2+x, 1/2-y'
' 1/2-y, 1/2+z, 1/2-x'
' 1/2+y, 1/2+x, 1/2+z'
' 1/2+x, 1/2+z, 1/2+y'
' 1/2+z, 1/2+y, 1/2+x'
' 1/2-x, 1/2-y, 1/2+z'
' 1/2-z, 1/2-x, 1/2+y'
' 1/2-y, 1/2-z, 1/2+x'
' 1/2+y, 1/2-x, 1/2-z'
' 1/2+x, 1/2-z, 1/2-y'
' 1/2+z, 1/2-y, 1/2-x'

_symmetry_cell_setting           cubic
_symmetry_space_group_name_H-M   'I -4 3 m'
_symmetry_space_group_name_Hall  'I -4 2 3'

_cell_length_a                   10.32120(3)
_cell_length_b                   10.32120(3)
_cell_length_c                   10.32120(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1099.490(8)
_cell_formula_units_Z            2


#------------------ CRYSTAL INFORMATION -------------------------------------#

_pd_spec_size_axial              ? # mm
_pd_spec_size_equat              0.015 # mm
_pd_spec_size_thick              0.03 # mm

_pd_spec_mounting                
;
packed powder in silica glass capillary
;
_pd_spec_mount_mode              
;
Debye-Scherrer, ID22 beamline-specific
;
_pd_spec_shape                   cylindrical
_pd_char_particle_morphology     ?
_pd_char_colour                  ?

#_pd_prep_conditions               ?
#_pd_prep_cool_rate                ? # K/min
#_pd_prep_pressure                 ? # kPa
#_pd_prep_temperature              ? # K

_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    5.0334
_exptl_crystal_density_method    ?
_exptl_crystal_F_000             1520
_exptl_absorpt_coefficient_mu    7.28

#------------------ DATA COLLECTION INFORMATION -----------------------------#

_cell_measurement_temperature    293
_cell_measurement_reflns_used    443
_cell_measurement_theta_min      1.00
_cell_measurement_theta_max      20.00

_diffrn_ambient_temperature      293
_diffrn_source_power             ?
_diffrn_source_voltage           ?
_diffrn_source_current           ?
_diffrn_radiation_source         'ESRF, ID22'
_diffrn_measurement_device_type  
;
High-resolution powder diffractometer
;
_diffrn_radiation_detector       2D-detector
_diffrn_radiation_monochromator  Si-111
_diffrn_radiation_probe          'synchrotron X-ray'

_diffrn_radiation_wavelength     0.354600
_diffrn_radiation_type           synchrotron

_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       1
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         1.00
_diffrn_reflns_theta_max         20.00


#------------------ COMPUTER PROGRAMS USED ----------------------------------#

_computing_data_collection       ?
_computing_cell_refinement       WinCSD
_computing_data_reduction        WinCSD
_computing_structure_solution    WinCSD
_computing_structure_refinement  WinCSD
_computing_molecular_graphics    ?
_computing_publication_material  'WinCSD (Akselrud et al, 1993)'

#### PLEASE do not forget the following reference :
#L. Akselrud, Yu. Grin.
#WinCSD: software package for crystallographic calculations (Version 4).
#J. Appl. Crystallogr., 2014, 47.

#------------------ REFINEMENT INFORMATION ----------------------------------#

# Use this field to give any special details about
# about the processing of the powder pattern
_pd_proc_ls_special_details      
; ?
;

# The next two items are given as text
_pd_proc_ls_profile_function     pseudo-Voigt
_pd_proc_ls_pref_orient_corr     ?
_pd_proc_ls_prof_R_factor        0.0258
_pd_proc_ls_prof_wR_factor       0.0371
_pd_proc_ls_prof_wR_expected     0.0620
_refine_ls_R_I_factor            0.0482
_refine_ls_goodness_of_fit_all   1.010
_refine_ls_R_factor_all          ?

_refine_special_details          
; ?
;

_refine_ls_structure_factor_coef Inet
_refine_ls_matrix_type           fullcycle

_refine_ls_weighting_scheme      unit
_refine_ls_weighting_details     1/[Yi+σ(Yi)]
_refine_ls_hydrogen_treatment    ?
_refine_ls_extinction_method     ?
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details ?
_refine_ls_abs_structure_Flack   ?
_refine_ls_number_reflns         443
_refine_ls_number_parameters     11
_refine_ls_number_restraints     ?
_refine_ls_number_constraints    ?
_refine_ls_restrained_S_all      ?
_refine_ls_restrained_S_obs      ?
_refine_ls_shift/su_max          ?
_refine_ls_shift/su_mean         ?

_refine_diff_density_max         1.29
_refine_diff_density_min         -0.66

#------------------ ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS --------#

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_thermal_displace_type
_atom_site_B_iso_or_equiv
_atom_site_symmetry_multiplicity
_atom_site_occupancy
Cu1 CU 0.25 0.5 0 Biso 1.792(10) 12 1.0
Cu2 CU 0.02033(5) 0.02033 0.78232(5) Biso 2.69(2) 24 0.5
Sb SB 0.26873(1) 0.26873 0.26873 Biso 1.343(4) 8 1.0
S1 S 0 0 0 Biso 2.01(5) 2 1.0
S2 S 0.11573(4) 0.11573 0.36294(5) Biso 1.203(9) 24 1.0

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
Cu1 S2 2.3126(5) 3_555 yes
Cu1 Sb 3.6644(2) . yes
Cu2 Cu2 0.5937(7) 10_555 yes
Cu2 S1 2.2662(5) 1_556 yes
Cu2 S2 2.2781(7) 4_556 yes
Cu2 Cu2 2.8803(7) 6_656 yes
Cu2 Sb 3.0819(6) 34_555 yes
Cu2 Cu2 3.2185(7) 5_546 yes
Cu2 Cu2 3.4741(7) 2_456 yes
Cu2 Sb 3.6752(6) 25_445 yes
Sb S2 2.4358(5) . yes
S2 S2 3.3785(6) 10_555 yes
S2 S2 3.6084(7) 2_555 yes

# start Validation Reply Form
_vrf_GEOM006_Cu11.5Ni0.5Sb4S13   
;
PROBLEM: _geom_angle_atom_site_label_2 is missing
RESPONSE: "inorganic structure"
;
_vrf_GEOM007_Cu11.5Ni0.5Sb4S13   
;
PROBLEM: _geom_angle_atom_site_label_3 is missing
RESPONSE: "inorganic structure"
;
_vrf_GEOM008_Cu11.5Ni0.5Sb4S13   
;
PROBLEM: _geom_angle is missing
RESPONSE: "inorganic structure"
;
_vrf_WEIGH01_Cu11.5Ni0.5Sb4S13   
;
PROBLEM: Unit weights are not acceptable for submissions to Acta
RESPONSE: "not Acta-journal submission"
;
####################################################################### 
# 
# 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_CuNi11p95Ni0p05Sb4S13
_database_code_depnum_ccdc_archive 'CCDC 2516850'
loop_
_audit_author_name
_audit_author_address
'Roman Gumeniuk'
;TU Bergakademie Freiberg
Germany
;
_audit_update_record             
;
2025-12-17 deposited with the CCDC.	2026-05-05 downloaded from the CCDC.
;

#------------------  SECTION 2. COMPOUND(S) DETAILS -------------------------#

_audit_creation_date             ?
_audit_creation_method           'WinCSD program'

#------------------ CHEMICAL INFORMATION ------------------------------------#

_chemical_formula_moiety         'Cu11.95 Ni0.05 S13 Sb4'
_chemical_formula_sum            'Cu11.95 Ni0.05 S13 Sb4'
_chemical_formula_weight         1666.31
_chemical_melting_point          ?
_chemical_compound_source        synthetic

loop_
_atom_type_symbol
_atom_type_description
_atom_type_number_in_cell
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
CU Cu 47.80 .125 .419 WinCSD
NI Ni .20 .207 .372 WinCSD
SB Sb 16.00 -.816 3.315 WinCSD
S S 52.00 .026 .048 WinCSD

#------------------ UNIT CELL INFORMATION -----------------------------------#

loop_
_symmetry_equiv_pos_as_xyz
' x, y, z'
'-y, x, -z'
'-x, -y, z'
' y, -x, -z'
'-x, y, 1/2+z'
' y, x, 1/2-z'
' x, -y, 1/2+z'
'-y, -x, 1/2-z'

_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_H-M   'P -4 c 2'
_symmetry_space_group_name_Hall  'P -4 -2 c'


_cell_length_a                   14.6010(1)
_cell_length_b                   14.6010(1)
_cell_length_c                   10.2731(1)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     2190.13(6)
_cell_formula_units_Z            4


#------------------ CRYSTAL INFORMATION -------------------------------------#

_pd_spec_size_axial              ? # mm
_pd_spec_size_equat              0.015 # mm
_pd_spec_size_thick              0.03 # mm

_pd_spec_mounting                
;
packed powder in silica glass capillary
;
_pd_spec_mount_mode              
;
Debye-Scherrer, ID22 beamline-specific
;
_pd_spec_shape                   cylindrical
_pd_char_particle_morphology     ?
_pd_char_colour                  ?

#_pd_prep_conditions               ?
#_pd_prep_cool_rate                ? # K/min
#_pd_prep_pressure                 ? # kPa
#_pd_prep_temperature              ? # K

_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    5.0530
_exptl_crystal_density_method    ?
_exptl_crystal_F_000             1520
_exptl_absorpt_coefficient_mu    7.31

#------------------ DATA COLLECTION INFORMATION -----------------------------#

_cell_measurement_temperature    25
_cell_measurement_reflns_used    1967
_cell_measurement_theta_min      1.00
_cell_measurement_theta_max      20.00

_diffrn_ambient_temperature      25
_diffrn_source_power             ?
_diffrn_source_voltage           ?
_diffrn_source_current           ?
_diffrn_radiation_source         'ESRF, ID22'
_diffrn_measurement_device_type  
;
High-resolution powder diffractometer
;
_diffrn_radiation_detector       2D-detector
_diffrn_radiation_monochromator  Si-111
_diffrn_radiation_probe          'synchrotron X-ray'

_diffrn_radiation_wavelength     0.354600
_diffrn_radiation_type           synchrotron

_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         1.00
_diffrn_reflns_theta_max         20.00


#------------------ COMPUTER PROGRAMS USED ----------------------------------#

_computing_data_collection       ?
_computing_cell_refinement       WinCSD
_computing_data_reduction        WinCSD
_computing_structure_solution    WinCSD
_computing_structure_refinement  WinCSD
_computing_molecular_graphics    ?
_computing_publication_material  'WinCSD (Akselrud et al, 1993)'

#### PLEASE do not forget the following reference :
#L. Akselrud, Yu. Grin.
#WinCSD: software package for crystallographic calculations (Version 4).
#J. Appl. Crystallogr., 2014, 47.

#------------------ REFINEMENT INFORMATION ----------------------------------#

# Use this field to give any special details about
# about the processing of the powder pattern
_pd_proc_ls_special_details      
; ?
;

# The next two items are given as text
_pd_proc_ls_profile_function     pseudo-Voigt
_pd_proc_ls_pref_orient_corr     ?
_pd_proc_ls_prof_R_factor        0.0418
_pd_proc_ls_prof_wR_factor       0.0639
_pd_proc_ls_prof_wR_expected     0.0562
_refine_ls_R_I_factor            0.0424
_refine_ls_goodness_of_fit_all   1.010
_refine_ls_R_factor_all          ?

_refine_special_details          
; ?
;

_refine_ls_structure_factor_coef Inet
_refine_ls_matrix_type           fullcycle

_refine_ls_weighting_scheme      unit
_refine_ls_weighting_details     1/[Yi+σ(Yi)]
_refine_ls_hydrogen_treatment    ?
_refine_ls_extinction_method     ?
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details ?
_refine_ls_abs_structure_Flack   ?
_refine_ls_number_reflns         1967
_refine_ls_number_parameters     59
_refine_ls_number_restraints     ?
_refine_ls_number_constraints    ?
_refine_ls_restrained_S_all      ?
_refine_ls_restrained_S_obs      ?
_refine_ls_shift/su_max          ?
_refine_ls_shift/su_mean         ?

_refine_diff_density_max         2.47
_refine_diff_density_min         -1.94

#------------------ ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS --------#

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_thermal_displace_type
_atom_site_B_iso_or_equiv
_atom_site_symmetry_multiplicity
_atom_site_occupancy
Cu1 CU 0.5 0.5 0 Biso 0.847(6) 2 1.0
Cu2 CU 0 0 0 Biso 0.880(6) 2 1.0
Cu3 CU 0.1376(2) 0.1376 0.75 Biso 0.756(6) 4 1.0
Cu4 CU 0.3796(2) 0.3796 0.75 Biso 0.712(6) 4 1.0
Cu5 CU 0 0.5 0.0245(4) Biso 0.783(6) 4 1.0
Cu6 CU 0.3522(2) 0.35222 0.25 Biso 0.919(6) 4 0.95(1)
Cu6 NI 0.3522(2) 0.35222 0.25 Biso 0.919(6) 4 0.05(1)
Cu7 CU 0.1264(2) 0.12646 0.25 Biso 0.866(6) 4 1.0
Cu8 CU 0.6248(2) 0.1214(2) 0.2401(3) Biso 0.617(6) 8 1.0
Cu9 CU 0.3620(2) 0.1507(2) 0.2162(2) Biso 0.988(6) 8 1.0
Cu10 CU 0.2717(1) 0.2496(2) 0.0419(2) Biso 0.974(6) 8 1.0
Sb1 SB 0.2537(1) 0.47731(6) 0.0242(1) Biso 0.573(5) 8 1.0
Sb2 SB 0.2562(1) 0.00708(6) 0.00784(10) Biso 0.513(5) 8 1.0
S1 S 0.2325(2) 0.23255 0.25 Biso 0.972(6) 4 1.0
S2 S 0.2501(4) 0.1472(3) 0.5987(4) Biso 0.845(6) 8 1.0
S3 S 0.2505(5) 0.6284(3) 0.1218(4) Biso 0.790(6) 8 1.0
S4 S 0.0161(4) 0.3718(4) 0.1526(6) Biso 0.851(6) 8 1.0
S5 S 0.0012(3) 0.1225(5) 0.1369(6) Biso 0.876(6) 8 1.0
S6 S 0.4848(3) 0.3725(5) 0.1336(6) Biso 0.833(6) 8 1.0
S7 S 0.4941(3) 0.1250(5) 0.1176(5) Biso 0.825(6) 8 1.0

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
Cu1 S6 2.324(6) . yes
Cu1 Sb1 3.619(2) . yes
Cu2 S5 2.277(6) . yes
Cu2 Sb2 3.743(2) . yes
Cu3 S2 2.266(6) . yes
Cu3 S5 2.347(5) 4_556 yes
Cu3 Cu8 3.479(4) 4_566 yes
Cu3 Sb2 3.694(2) 1_556 yes
Cu3 Sb2 3.695(2) 2_556 yes
Cu4 S3 2.302(6) 2_656 yes
Cu4 S6 2.314(6) 4_566 yes
Cu4 Sb1 3.622(2) 2_656 yes
Cu4 Sb1 3.653(2) 1_556 yes
Cu5 S4 2.300(6) . yes
Cu5 S7 2.340(7) 2_555 yes
Cu5 Cu8 3.509(4) 6_555 yes
Cu5 Sb2 3.577(2) 2_555 yes
Cu5 Sb1 3.720(2) . yes
Cu6 S6 2.295(6) . yes
Cu6 S1 2.471(4) . yes
Cu6 Cu10 2.862(3) . yes
Cu6 Cu9 2.965(3) . yes
Cu6 Sb1 3.284(2) . yes
Cu7 S5 2.166(5) . yes
Cu7 S1 2.191(4) . yes
Cu7 Cu9 3.476(3) . yes
Cu7 Cu10 3.507(3) . yes
Cu7 Sb2 3.580(2) . yes
Cu7 Sb2 3.796(2) 2_555 yes
Cu8 S7 2.286(6) . yes
Cu8 S4 2.292(6) 8_655 yes
Cu8 S3 2.359(6) 6_555 yes
Cu8 S2 2.363(6) 5_654 yes
Cu8 Sb2 3.498(3) 3_655 yes
Cu8 Sb1 3.651(3) 2_655 yes
Cu8 Sb2 3.657(3) 5_655 yes
Cu8 Sb1 3.772(3) 6_555 yes
Cu9 S7 2.210(5) . yes
Cu9 S1 2.264(4) . yes
Cu9 S4 2.387(6) 6_555 yes
Cu9 Cu10 2.651(3) . yes
Cu9 Sb2 3.372(2) . yes
Cu9 Cu10 3.462(3) 6_555 yes
Cu9 Sb1 3.493(2) 6_555 yes
Cu9 Sb1 3.723(2) 2_655 yes
Cu10 S1 2.226(2) . yes
Cu10 S3 2.226(5) 2_655 yes
Cu10 S2 2.323(5) 6_555 yes
Cu10 Sb1 3.340(3) . yes
Cu10 Sb2 3.566(3) . yes
Cu10 Sb1 3.727(2) 2_655 yes
Sb1 S7 2.414(6) 4_565 yes
Sb1 S3 2.424(5) . yes
Sb1 S6 2.438(6) 4_565 yes
Sb1 S6 3.873(5) . yes
Sb1 S2 3.875(6) 6_555 yes
Sb1 S6 3.921(6) 6_555 yes
Sb2 S4 2.384(6) 4_555 yes
Sb2 S2 2.440(5) 7_554 yes
Sb2 S5 2.457(7) 4_555 yes
Sb2 S4 3.877(6) 6_555 yes
S2 S3 3.284(7) 7_565 yes
S2 S4 3.672(7) 6_555 yes
S2 S3 3.696(7) 2_656 yes
S3 S7 3.551(8) 4_565 yes
S3 S6 3.577(8) 4_565 yes
S3 S3 3.631(7) 8_665 yes
S4 S7 3.359(8) 6_555 yes
S4 S5 3.650(9) . yes
S4 S7 3.694(8) 8_565 yes
S5 S5 3.416(8) 6_555 yes
S5 S5 3.455(8) 8_555 yes
S5 S5 3.580(9) 3_555 yes
S6 S6 3.332(8) 6_555 yes
S6 S7 3.619(9) . yes
S7 S7 3.656(9) 3_655 yes

# start Validation Reply Form
_vrf_GEOM006_CuNi11.95Ni0.05Sb4S13 
;
PROBLEM: _geom_angle_atom_site_label_2 is missing
RESPONSE: "inorganic structure"
;
_vrf_GEOM007_CuNi11.95Ni0.05Sb4S13 
;
PROBLEM: _geom_angle_atom_site_label_3 is missing
RESPONSE: "inorganic structure"
;
_vrf_GEOM008_CuNi11.95Ni0.05Sb4S13 
;
PROBLEM: _geom_angle is missing
RESPONSE: "inorganic structure"
;
_vrf_LABEL01_CuNi11.95Ni0.05Sb4S13 
;
PROBLEM: An _atom_site_label occurs more than once in the atom list.
RESPONSE: "statistical mixture"
;
_vrf_WEIGH01_CuNi11.95Ni0.05Sb4S13 
;
PROBLEM: Unit weights are not acceptable for submissions to Acta
RESPONSE: "not Acta-journal submission"
;
####################################################################### 
# 
# 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_Cu11p8Ni0p2Sb4S13_CCDC1
_database_code_depnum_ccdc_archive 'CCDC 2516848'
loop_
_audit_author_name
_audit_author_address
'Roman Gumeniuk'
;TU Bergakademie Freiberg
Germany
;
_audit_update_record             
;
2025-12-17 deposited with the CCDC.	2026-05-05 downloaded from the CCDC.
;

#------------------  SECTION 2. COMPOUND(S) DETAILS -------------------------#

_audit_creation_date             ?
_audit_creation_method           'WinCSD program'

#------------------ CHEMICAL INFORMATION ------------------------------------#

_chemical_formula_moiety         'Cu11.8 Ni0.2 S13 Sb4'
_chemical_formula_sum            'Cu11.8 Ni0.2 S13 Sb4'
_chemical_formula_weight         1665.62
_chemical_melting_point          ?
_chemical_compound_source        synthetic

loop_
_atom_type_symbol
_atom_type_description
_atom_type_number_in_cell
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
CU Cu 48.00 .125 .419 WinCSD
SB Sb 16.00 -.816 3.315 WinCSD
S S 52.00 .026 .048 WinCSD

#------------------ UNIT CELL INFORMATION -----------------------------------#

loop_
_symmetry_equiv_pos_as_xyz
' x, y, z'
'-y, x, -z'
'-x, -y, z'
' y, -x, -z'
'-x, y, 1/2+z'
' y, x, 1/2-z'
' x, -y, 1/2+z'
'-y, -x, 1/2-z'

_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_H-M   'P -4 c 2'
_symmetry_space_group_name_Hall  'P -4 -2c'


_cell_length_a                   14.5903(4)
_cell_length_b                   14.5903(4)
_cell_length_c                   10.2822(4)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     2188.8(2)
_cell_formula_units_Z            4


#------------------ CRYSTAL INFORMATION -------------------------------------#

_pd_spec_size_axial              ? # mm
_pd_spec_size_equat              0.015 # mm
_pd_spec_size_thick              0.03 # mm

_pd_spec_mounting                
;
packed powder in silica glass capillary
;
_pd_spec_mount_mode              
;
Debye-Scherrer, ID22 beamline-specific
;
_pd_spec_shape                   cylindrical
_pd_char_particle_morphology     ?
_pd_char_colour                  ?

#_pd_prep_conditions               ?
#_pd_prep_cool_rate                ? # K/min
#_pd_prep_pressure                 ? # kPa
#_pd_prep_temperature              ? # K

_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    5.0567
_exptl_crystal_density_method    ?
_exptl_crystal_F_000             3040
_exptl_absorpt_coefficient_mu    7.32

#------------------ DATA COLLECTION INFORMATION -----------------------------#

_cell_measurement_temperature    10
_cell_measurement_reflns_used    4428
_cell_measurement_theta_min      1.00
_cell_measurement_theta_max      20.00

_diffrn_ambient_temperature      10
_diffrn_source_power             ?
_diffrn_source_voltage           ?
_diffrn_source_current           ?
_diffrn_radiation_source         'ESRF, ID22'
_diffrn_measurement_device_type  
;
High-resolution powder diffractometer
;
_diffrn_radiation_detector       2D-detector
_diffrn_radiation_monochromator  Si-111
_diffrn_radiation_probe          'synchrotron X-ray'

_diffrn_radiation_wavelength     0.354600
_diffrn_radiation_type           synchrotron


_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         1.00
_diffrn_reflns_theta_max         20.00


#------------------ COMPUTER PROGRAMS USED ----------------------------------#

_computing_data_collection       ?
_computing_cell_refinement       WinCSD
_computing_data_reduction        WinCSD
_computing_structure_solution    WinCSD
_computing_structure_refinement  WinCSD
_computing_molecular_graphics    ?
_computing_publication_material  'WinCSD (Akselrud et al, 1993)'

#### PLEASE do not forget the following reference :
#L. Akselrud, Yu. Grin.
#WinCSD: software package for crystallographic calculations (Version 4).
#J. Appl. Crystallogr., 2014, 47.

#------------------ REFINEMENT INFORMATION ----------------------------------#

# Use this field to give any special details about
# about the processing of the powder pattern
_pd_proc_ls_special_details      
; ?
;

# The next two items are given as text
_pd_proc_ls_profile_function     pseudo-Voigt
_pd_proc_ls_pref_orient_corr     
; Preffered orientation was refined using WinCSD
formula (Pecharskii, Akselrud & Zavalii, 1987):

I~corr~=I~obs~/[1+(\t^2^-1)^.^sin^2^\f]^1/2^

'Axis'  1  0  0, \t=1.000

;

#PLEASE do not forget the following reference :
#L. Akselrud, Yu. Grin.
#J. Appl. Crystallogr., 2014, 47.

_pd_proc_ls_prof_R_factor        0.0616
_pd_proc_ls_prof_wR_factor       0.0918
_pd_proc_ls_prof_wR_expected     0.1492
_refine_ls_R_I_factor            0.0417
_refine_ls_goodness_of_fit_all   1.010
_refine_ls_R_factor_all          ?

_refine_special_details          
; ?
;

_refine_ls_structure_factor_coef Inet
_refine_ls_matrix_type           fullcycle

_refine_ls_weighting_scheme      unit
_refine_ls_weighting_details     1/[Yi+σ(Yi)]
_refine_ls_hydrogen_treatment    ?
_refine_ls_extinction_method     ?
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details ?
_refine_ls_abs_structure_Flack   ?
_refine_ls_number_reflns         4428
_refine_ls_number_parameters     40
_refine_ls_number_restraints     ?
_refine_ls_number_constraints    ?
_refine_ls_restrained_S_all      ?
_refine_ls_restrained_S_obs      ?
_refine_ls_shift/su_max          ?
_refine_ls_shift/su_mean         ?

_refine_diff_density_max         3.47
_refine_diff_density_min         -2.05

#------------------ ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS --------#

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_thermal_displace_type
_atom_site_B_iso_or_equiv
_atom_site_symmetry_multiplicity
_atom_site_occupancy
Cu1 CU 0.5 0.5 0 Biso 0.60(15) 2 1.0
Cu2 CU 0 0 0 Biso 0.6(2) 2 1.0
Cu3 CU 0.1347(6) 0.13474 0.75 Biso 0.57(10) 4 1.0
Cu4 CU 0.3780(7) 0.37801 0.75 Biso 0.46(10) 4 1.0
Cu5 CU 0 0.5 0.018(2) Biso 0.77(13) 4 1.0
Cu6 CU 0.3546(6) 0.35466 0.25 Biso 0.95(9) 4 1.0
Cu7 CU 0.1284(6) 0.12843 0.25 Biso 0.75(8) 4 1.0
Cu8 CU 0.6245(7) 0.1240(7) 0.243(1) Biso 0.59(7) 8 1.0
Cu9 CU 0.3592(6) 0.1520(6) 0.2223(8) Biso 0.88(7) 8 1.0
Cu10 CU 0.2694(5) 0.2521(6) 0.0427(7) Biso 0.73(6) 8 1.0
Sb1 SB 0.2514(4) 0.4786(3) 0.0218(4) Biso 0.47(3) 8 1.0
Sb2 SB 0.2548(4) 0.0092(2) 0.0114(4) Biso 0.46(3) 8 1.0
S1 S 0.2340(7) 0.23408 0.25 Biso 0.87(15) 4 1.0
S2 S 0.250(2) 0.144(2) 0.601(2) Biso 0.56(13) 8 1.0
S3 S 0.250(2) 0.629(1) 0.119(2) Biso 0.47(12) 8 1.0
S4 S 0.017(2) 0.371(2) 0.152(2) Biso 0.53(14) 8 1.0
S5 S 0.005(1) 0.119(2) 0.132(3) Biso 0.67(14) 8 1.0
S6 S 0.486(2) 0.373(2) 0.131(3) Biso 0.59(14) 8 1.0
S7 S 0.490(2) 0.123(2) 0.125(2) Biso 0.7(2) 8 1.0


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
Cu1 S6 2.29(2) . yes
Cu1 Sb1 3.647(6) . yes
Cu2 S5 2.22(2) . yes
Cu2 Sb2 3.722(5) . yes
Cu3 S2 2.28(2) . yes
Cu3 S5 2.38(2) 4_556 yes
Cu3 Cu8 3.516(14) 4_566 yes
Cu3 Sb2 3.674(8) 2_556 yes
Cu3 Sb2 3.694(7) 1_556 yes
Cu4 S3 2.29(2) 2_656 yes
Cu4 S6 2.33(2) 4_566 yes
Cu4 Sb1 3.645(9) 2_656 yes
Cu4 Sb1 3.659(8) 1_556 yes
Cu5 S4 2.34(2) . yes
Cu5 S7 2.34(3) 2_555 yes
Cu5 Cu8 3.546(14) 6_555 yes
Cu5 Sb2 3.593(5) 2_555 yes
Cu5 Sb1 3.681(6) . yes
Cu6 S6 2.29(2) . yes
Cu6 S1 2.488(14) . yes
Cu6 Cu10 2.885(10) . yes
Cu6 Cu9 2.971(12) . yes
Cu6 Sb1 3.323(8) . yes
Cu7 S5 2.17(2) . yes
Cu7 S1 2.180(14) . yes
Cu7 Cu9 3.397(12) . yes
Cu7 Cu10 3.468(10) . yes
Cu7 Sb2 3.527(7) . yes
Cu7 Sb2 3.829(7) 2_555 yes
Cu8 S7 2.30(2) . yes
Cu8 S3 2.33(2) 6_555 yes
Cu8 S4 2.33(2) 8_655 yes
Cu8 S2 2.35(2) 5_654 yes
Cu8 Sb2 3.544(11) 3_655 yes
Cu8 Sb1 3.626(11) 2_655 yes
Cu8 Sb2 3.676(11) 5_655 yes
Cu8 Sb1 3.717(11) 6_555 yes
Cu9 S7 2.19(2) . yes
Cu9 S1 2.201(13) . yes
Cu9 S4 2.35(2) 6_555 yes
Cu9 Cu10 2.694(11) . yes
Cu9 Cu10 3.348(11) 6_555 yes
Cu9 Sb2 3.371(9) . yes
Cu9 Sb1 3.472(9) 6_555 yes
Cu9 Sb1 3.742(9) 2_655 yes
Cu10 S1 2.208(7) . yes
Cu10 S3 2.23(2) 2_655 yes
Cu10 S2 2.35(2) 6_555 yes
Cu10 Sb1 3.323(10) . yes
Cu10 Sb2 3.565(10) . yes
Cu10 Sb1 3.735(8) 2_655 yes
Sb1 S3 2.42(2) . yes
Sb1 S6 2.43(3) 4_565 yes
Sb1 S7 2.45(2) 4_565 yes
Sb1 S2 3.89(2) 6_555 yes
Sb1 S6 3.92(2) . yes
Sb2 S2 2.43(2) 7_554 yes
Sb2 S4 2.43(2) 4_555 yes
Sb2 S5 2.47(3) 4_555 yes
Sb2 S4 3.85(2) 6_555 yes
S2 S3 3.30(3) 7_565 yes
S2 S4 3.66(3) 6_555 yes
S2 S5 3.68(3) 6_555 yes
S2 S3 3.70(3) 2_656 yes
S3 S6 3.57(3) 4_565 yes
S3 S7 3.58(3) 4_565 yes
S3 S3 3.65(3) 8_665 yes
S4 S7 3.25(3) 6_555 yes
S4 S7 3.68(3) 8_565 yes
S4 S5 3.69(3) . yes
S5 S5 3.39(3) 6_555 yes
S5 S5 3.50(3) 3_555 yes
S5 S5 3.54(3) 8_555 yes
S5 S5 3.68(3) 2_555 yes
S6 S6 3.37(3) 6_555 yes
S6 S7 3.65(4) . yes
S7 S7 3.62(4) 3_655 yes

# start Validation Reply Form
_vrf_GEOM006_Cu11.8Ni0.2Sb4S13   
;
PROBLEM: _geom_angle_atom_site_label_2 is missing
RESPONSE: "inorganic structure"
;
_vrf_GEOM007_Cu11.8Ni0.2Sb4S13   
;
PROBLEM: _geom_angle_atom_site_label_3 is missing
RESPONSE: "inorganic structure"
;
_vrf_GEOM008_Cu11.8Ni0.2Sb4S13   
;
PROBLEM: _geom_angle is missing
RESPONSE: "inorganic structure"
;
_vrf_WEIGH01_Cu11.8Ni0.2Sb4S13   
;
PROBLEM: Unit weights are not acceptable for submissions to Acta
RESPONSE: "not Acta-journal submission"
;
