Synthesis Examples
Each file on this page was generated at the corresponding checkpoint in the walkthrough script.
Initial Synthesis (FOS)
fos_id: TE001
fos_type: synthesis
// This comment will stay attached to the description when saving
// (Until comments are cleared)
description: My First Synthesis
// ! Comments starting with a ! do not get read from the file.
group_id: kovnir-0000-0003-1152-1912
project_id: travis5672/clathrates/Ba2-TM5-Sb6
[Experimenters]
name: Travis Errthum
affiliation: Kovnir Group - Iowa State University
orcid: 0009-0006-1937-5672
// Single brackets on a header mean there is only one group
[Reaction]
nominal_formula: Ba2Zn5Sb6
nominal_amount: 250.0
nominal_amount_unit: mg
[Products]
name: Barium Zinc Antimonide (2-5-6)
formula: Ba2Zn5Sb6
expected: true
obtained: true
expected_amount: 250.0
expected_amount_unit: mg
obtained_amount: 200.0
obtained_amount_unit: mg
observations: Black Powder
characterizations: PXRD, EDS, Eyeballs
structure_comments: [;;;
Unique clathrate with novel polyhedra.
Space group Pnma]
// Double brackets on a header mean there are multiple similar groups
[[Materials]]
:name
:type
:formula
:supplier
:cas
:form
:purity
:env
:amount
:amount_unit
Barium
reagent
Ba
Thermofisher
7440-39-3
lump
0.999
Ar (g)
// The comment below will be correctly re-calculated using a calc_routine
// ! Total weight percent: 200%
2.0
mol ratio
// Similar to headers, single brackets mean there is only one group,
// in this case for treatments of Barium
treatments: [
type: cutting
repeats: 1
observations: smaller pieces improve homogenization
]
Zinc
reagent
Zn
Sigma Aldrich
7440-66-6
powder
0.995
Ar (g)
5.0
mol ratio
Antimony
reagent
Sb
Chem Stores?
7440-36-0
powder
0.999
Ar (g)
6.0
mol ratio
// This is a comment on the treatments block
[[Treatments]]
:type
:repeats
:observations
weigh
1
// The syntax below allows me to use multiple lines for longer texts.
[;;;
Weighed stoichiometrically to carbonized ampoule.
Barium added last to avoid contact with ampoule
during reaction]
recovered_mass: 250.0
seal
1
Evacuated ampoule and sealed with H2/O2 torch
anneal
2
Opened under argon atmosphere and ground well before sealing in new ampoule in between annealings.
start_temp: 25
start_temp_unit: C
// Here, the double brackets signal that there are multiple program sections.
program: [[
type: ramp
temp: 600
time: 10
temp_unit: C
time_unit: h
type: dwell
time: 120
time_unit: h
]]
grind
3
dark gray powder now
recovered_mass: 200.0
[CIFs]
file_name: Ba2Zn5Sb6_ICSD
extension: .cif
embedded: {{{
#(C) 2025 by FIZ Karlsruhe - Leibniz Institute for Information Infrastructure. All rights reserved.
data_71031-ICSD
_database_code_ICSD 71031
_audit_creation_date 2023-08-01
_chemical_name_common 'Barium zinc antimonide (2/5/6)'
_chemical_formula_structural 'Ba2 Zn5 Sb6'
_chemical_formula_sum 'Ba2 Sb6 Zn5'
_exptl_crystal_density_diffrn 6.13
_diffrn_ambient_temperature 100.
_citation_title
;
New trick for an old dog: from prediction to properties of hidden clathrates
\(Ba_2 Zn_5As_6\) and \(Ba_2 Zn_5Sb_6\)
;
loop_
_citation_id
_citation_journal_full
_citation_year
_citation_journal_volume
_citation_page_first
_citation_page_last
_citation_journal_id_ASTM
primary 'Journal of the American Chemical Society' 2023 145 4638 4646 JACSAT
loop_
_citation_author_citation_id
_citation_author_name
primary 'Yox, Philip'
primary 'Cerasoli, Frank'
primary 'Sarkar, Arka'
primary 'Kyveryga, Victoria'
primary 'Viswanathan, Gayatri'
primary 'Donadio, Davide'
primary 'Kovnir, Kirill'
_cell_length_a 11.4154(5)
_cell_length_b 10.0135(4)
_cell_length_c 12.6172(5)
_cell_angle_alpha 90
_cell_angle_beta 90
_cell_angle_gamma 90
_cell_volume 1442.24
_cell_formula_units_Z 4
_space_group_name_H-M_alt 'P m n a'
_space_group_IT_number 53
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 'x+1/2, y, -z+1/2'
2 'x+1/2, -y, z+1/2'
3 '-x, y, z'
4 '-x, -y, -z'
5 '-x+1/2, -y, z+1/2'
6 '-x+1/2, y, -z+1/2'
7 'x, -y, -z'
8 'x, y, z'
loop_
_atom_type_symbol
_atom_type_oxidation_number
Ba0+ 0
Sb0+ 0
Zn0+ 0
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_symmetry_multiplicity
_atom_site_Wyckoff_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_occupancy
Ba1 Ba0+ 4 h 0.5 0.23891(4) 0.64640(3) 0.00367(9) 1
Ba2 Ba0+ 4 g 0.75 0.71608(4) 0.75 0.00794(10) 1
Sb1 Sb0+ 4 f 0.32061(4) 0.5 0.5 0.00275(10) 1
Sb2 Sb0+ 4 h 0.5 0.86799(4) 0.61427(3) 0.00219(10) 1
Sb3 Sb0+ 4 h 0.5 0.73181(4) 0.93973(3) 0.00287(10) 1
Sb4 Sb0+ 8 i 0.19164(3) 0.10079(3) 0.65092(2) 0.00228(8) 1
Sb5 Sb0+ 4 h 0.5 0.50694(4) 0.80966(3) 0.00258(10) 1
Zn1 Zn0+ 4 h 0.5 0.94723(7) 0.81658(6) 0.00330(16) 1
Zn2 Zn0+ 4 e 0.33104(7) 0. 0.5 0.00356(16) 1
Zn3 Zn0+ 4 h 0.5 0.60202(7) 0.61084(6) 0.00339(16) 1
Zn4 Zn0+ 8 i 0.15880(5) 0.65041(5) 0.41232(4) 0.00452(13) 1
loop_
_atom_site_aniso_label
_atom_site_aniso_type_symbol
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_12
_atom_site_aniso_U_13
_atom_site_aniso_U_23
Ba1 Ba0+ 0.0056(2) 0.00269(19) 0.00270(18) 0. 0. -0.00066(15)
Ba2 Ba0+ 0.0031(2) 0.0110(2) 0.0097(2) 0. -0.00029(16) 0.
Sb1 Sb0+ 0.0025(2) 0.0026(2) 0.0031(2) 0. 0. 0.00002(17)
Sb2 Sb0+ 0.0037(2) 0.0013(2) 0.0015(2) 0. 0. -0.00028(17)
Sb3 Sb0+ 0.0053(2) 0.0017(2) 0.0016(2) 0. 0. -0.00002(17)
Sb4 Sb0+ 0.00259(16) 0.00227(16) 0.00198(14) 0.00013(12) 0.00028(12)
-0.00016(12)
Sb5 Sb0+ 0.0043(2) 0.0014(2) 0.0020(2) 0. 0. 0.00017(17)
Zn1 Zn0+ 0.0041(4) 0.0027(4) 0.0032(4) 0. 0. 0.0000(3)
Zn2 Zn0+ 0.0034(4) 0.0039(4) 0.0034(4) 0. 0. -0.0007(3)
Zn3 Zn0+ 0.0043(4) 0.0023(4) 0.0036(4) 0. 0. 0.0006(3)
Zn4 Zn0+ 0.0051(3) 0.0030(3) 0.0054(3) -0.0001(2) -0.0003(2) 0.0010(2)
#End of TTdata_71031-ICSD
#################### END FOS EMBED }}}
Initial Synthesis (JSON)
{
"metadata": {
"fos_id": "TE001",
"fos_type": "synthesis",
"description": "My First Synthesis",
"group_id": "kovnir-0000-0003-1152-1912",
"project_id": "travis5672/clathrates/Ba2-TM5-Sb6"
},
"experimenters": [
{
"name": "Travis Errthum",
"affiliation": "Kovnir Group - Iowa State University",
"orcid": "0009-0006-1937-5672"
}
],
"reaction": {
"nominal_formula": "Ba2Zn5Sb6",
"nominal_amount": "250.0",
"nominal_amount_unit": "milligram"
},
"products": [
{
"name": "Barium Zinc Antimonide (2-5-6)",
"formula": "Ba2Zn5Sb6",
"expected": "True",
"obtained": "True",
"expected_amount": "250.0",
"expected_amount_unit": "milligram",
"obtained_amount": "200.0",
"obtained_amount_unit": "milligram",
"observations": "Black Powder",
"characterizations": "PXRD, EDS, Eyeballs",
"structure_comments": "Unique clathrate with novel polyhedra. Space group Pnma"
}
],
"materials": [
{
"name": "Barium",
"type": "reagent",
"formula": "Ba",
"supplier": "Thermofisher",
"cas": "7440-39-3",
"form": "lump",
"purity": "0.999",
"env": "Ar (g)",
"amount": "2.0",
"amount_unit": "mol ratio",
"treatments": [
{
"type": "cutting",
"repeats": "1",
"observations": "smaller pieces improve homogenization"
}
]
},
{
"name": "Zinc",
"type": "reagent",
"formula": "Zn",
"supplier": "Sigma Aldrich",
"cas": "7440-66-6",
"form": "powder",
"purity": "0.995",
"env": "Ar (g)",
"amount": "5.0",
"amount_unit": "mol ratio"
},
{
"name": "Antimony",
"type": "reagent",
"formula": "Sb",
"supplier": "Chem Stores?",
"cas": "7440-36-0",
"form": "powder",
"purity": "0.999",
"env": "Ar (g)",
"amount": "6.0",
"amount_unit": "mol ratio"
}
],
"treatments": [
{
"type": "weigh",
"repeats": "1",
"observations": "Weighed stoichiometrically to carbonized ampoule. Barium added last to avoid contact with ampoule during reaction",
"recovered_mass": "250.0"
},
{
"type": "seal",
"repeats": "1",
"observations": "Evacuated ampoule and sealed with H2/O2 torch"
},
{
"type": "anneal",
"repeats": "2",
"observations": "Opened under argon atmosphere and ground well before sealing in new ampoule in between annealings.",
"start_temp": "25",
"start_temp_unit": "degree_Celsius",
"program": [
{
"type": "ramp",
"temp": "600",
"time": "10",
"temp_unit": "degree_Celsius",
"time_unit": "hour"
},
{
"type": "dwell",
"time": "120",
"time_unit": "hour"
}
]
},
{
"type": "grind",
"repeats": "3",
"observations": "dark gray powder now",
"recovered_mass": "200.0"
}
],
"cifs": [
{
"file_name": "Ba2Zn5Sb6_ICSD",
"extension": ".cif",
"embedded": [
"\n",
"#(C) 2025 by FIZ Karlsruhe - Leibniz Institute for Information Infrastructure. All rights reserved.\n",
"data_71031-ICSD\n",
"_database_code_ICSD 71031\n",
"_audit_creation_date 2023-08-01\n",
"_chemical_name_common 'Barium zinc antimonide (2/5/6)'\n",
"_chemical_formula_structural 'Ba2 Zn5 Sb6'\n",
"_chemical_formula_sum 'Ba2 Sb6 Zn5'\n",
"_exptl_crystal_density_diffrn 6.13\n",
"_diffrn_ambient_temperature 100.\n",
"_citation_title\n",
";\n",
"New trick for an old dog: from prediction to properties of hidden clathrates \n",
"\\(Ba_2 Zn_5As_6\\) and \\(Ba_2 Zn_5Sb_6\\)\n",
";\n",
"loop_\n",
"_citation_id\n",
"_citation_journal_full\n",
"_citation_year\n",
"_citation_journal_volume\n",
"_citation_page_first\n",
"_citation_page_last\n",
"_citation_journal_id_ASTM\n",
"primary 'Journal of the American Chemical Society' 2023 145 4638 4646 JACSAT\n",
"loop_\n",
"_citation_author_citation_id\n",
"_citation_author_name\n",
"primary 'Yox, Philip'\n",
"primary 'Cerasoli, Frank'\n",
"primary 'Sarkar, Arka'\n",
"primary 'Kyveryga, Victoria'\n",
"primary 'Viswanathan, Gayatri'\n",
"primary 'Donadio, Davide'\n",
"primary 'Kovnir, Kirill'\n",
"_cell_length_a 11.4154(5)\n",
"_cell_length_b 10.0135(4)\n",
"_cell_length_c 12.6172(5)\n",
"_cell_angle_alpha 90\n",
"_cell_angle_beta 90\n",
"_cell_angle_gamma 90\n",
"_cell_volume 1442.24\n",
"_cell_formula_units_Z 4\n",
"_space_group_name_H-M_alt 'P m n a'\n",
"_space_group_IT_number 53\n",
"loop_\n",
"_space_group_symop_id\n",
"_space_group_symop_operation_xyz\n",
"1 'x+1/2, y, -z+1/2'\n",
"2 'x+1/2, -y, z+1/2'\n",
"3 '-x, y, z'\n",
"4 '-x, -y, -z'\n",
"5 '-x+1/2, -y, z+1/2'\n",
"6 '-x+1/2, y, -z+1/2'\n",
"7 'x, -y, -z'\n",
"8 'x, y, z'\n",
"loop_\n",
"_atom_type_symbol\n",
"_atom_type_oxidation_number\n",
"Ba0+ 0\n",
"Sb0+ 0\n",
"Zn0+ 0\n",
"loop_\n",
"_atom_site_label\n",
"_atom_site_type_symbol\n",
"_atom_site_symmetry_multiplicity\n",
"_atom_site_Wyckoff_symbol\n",
"_atom_site_fract_x\n",
"_atom_site_fract_y\n",
"_atom_site_fract_z\n",
"_atom_site_U_iso_or_equiv\n",
"_atom_site_occupancy\n",
"Ba1 Ba0+ 4 h 0.5 0.23891(4) 0.64640(3) 0.00367(9) 1\n",
"Ba2 Ba0+ 4 g 0.75 0.71608(4) 0.75 0.00794(10) 1\n",
"Sb1 Sb0+ 4 f 0.32061(4) 0.5 0.5 0.00275(10) 1\n",
"Sb2 Sb0+ 4 h 0.5 0.86799(4) 0.61427(3) 0.00219(10) 1\n",
"Sb3 Sb0+ 4 h 0.5 0.73181(4) 0.93973(3) 0.00287(10) 1\n",
"Sb4 Sb0+ 8 i 0.19164(3) 0.10079(3) 0.65092(2) 0.00228(8) 1\n",
"Sb5 Sb0+ 4 h 0.5 0.50694(4) 0.80966(3) 0.00258(10) 1\n",
"Zn1 Zn0+ 4 h 0.5 0.94723(7) 0.81658(6) 0.00330(16) 1\n",
"Zn2 Zn0+ 4 e 0.33104(7) 0. 0.5 0.00356(16) 1\n",
"Zn3 Zn0+ 4 h 0.5 0.60202(7) 0.61084(6) 0.00339(16) 1\n",
"Zn4 Zn0+ 8 i 0.15880(5) 0.65041(5) 0.41232(4) 0.00452(13) 1\n",
"loop_\n",
"_atom_site_aniso_label\n",
"_atom_site_aniso_type_symbol\n",
"_atom_site_aniso_U_11\n",
"_atom_site_aniso_U_22\n",
"_atom_site_aniso_U_33\n",
"_atom_site_aniso_U_12\n",
"_atom_site_aniso_U_13\n",
"_atom_site_aniso_U_23\n",
"Ba1 Ba0+ 0.0056(2) 0.00269(19) 0.00270(18) 0. 0. -0.00066(15)\n",
"Ba2 Ba0+ 0.0031(2) 0.0110(2) 0.0097(2) 0. -0.00029(16) 0.\n",
"Sb1 Sb0+ 0.0025(2) 0.0026(2) 0.0031(2) 0. 0. 0.00002(17)\n",
"Sb2 Sb0+ 0.0037(2) 0.0013(2) 0.0015(2) 0. 0. -0.00028(17)\n",
"Sb3 Sb0+ 0.0053(2) 0.0017(2) 0.0016(2) 0. 0. -0.00002(17)\n",
"Sb4 Sb0+ 0.00259(16) 0.00227(16) 0.00198(14) 0.00013(12) 0.00028(12)\n",
"-0.00016(12)\n",
"Sb5 Sb0+ 0.0043(2) 0.0014(2) 0.0020(2) 0. 0. 0.00017(17)\n",
"Zn1 Zn0+ 0.0041(4) 0.0027(4) 0.0032(4) 0. 0. 0.0000(3)\n",
"Zn2 Zn0+ 0.0034(4) 0.0039(4) 0.0034(4) 0. 0. -0.0007(3)\n",
"Zn3 Zn0+ 0.0043(4) 0.0023(4) 0.0036(4) 0. 0. 0.0006(3)\n",
"Zn4 Zn0+ 0.0051(3) 0.0030(3) 0.0054(3) -0.0001(2) -0.0003(2) 0.0010(2)\n",
"#End of TTdata_71031-ICSD\n"
]
}
]
}
Checkpoint 1
fos_id: TE001
fos_type: synthesis
// This comment will stay attached to the description when saving
// (Until comments are cleared)
description: My First Synthesis
group_id: kovnir-0000-0003-1152-1912
project_id: travis5672/clathrates/Ba2-TM5-Sb6
[Experimenters]
name: Travis Errthum
affiliation: Kovnir Group - Iowa State University
orcid: 0009-0006-1937-5672
// Single brackets on a header mean there is only one group
[Reaction]
nominal_formula: Ba2Zn5Sb6
nominal_amount: 250.0
nominal_amount_unit: milligram
[Products]
name: Barium Zinc Antimonide (2-5-6)
formula: Ba2Zn5Sb6
expected: True
obtained: True
expected_amount: 250.0
expected_amount_unit: milligram
obtained_amount: 200.0
obtained_amount_unit: milligram
observations: Black Powder
characterizations: PXRD, EDS, Eyeballs
structure_comments: Unique clathrate with novel polyhedra. Space group Pnma
// Double brackets on a header mean there are multiple similar groups
[[Materials]]
:name
:type
:formula
:supplier
:cas
:form
:purity
:env
:amount
:amount_unit
Barium
reagent
Ba
Thermofisher
7440-39-3
lump
0.999
Ar (g)
// The comment below will be correctly re-calculated using a calc_routine
2.0
mol ratio
// Similar to headers, single brackets mean there is only one group,
// in this case for treatments of Barium
treatments: [
type: cutting
repeats: 1
observations: smaller pieces improve homogenization
]
Zinc
reagent
Zn
Sigma Aldrich
7440-66-6
powder
0.995
Ar (g)
5.0
mol ratio
Antimony
reagent
Sb
Chem Stores?
7440-36-0
powder
0.999
Ar (g)
6.0
mol ratio
// This is a comment on the treatments block
[[Treatments]]
:type
:repeats
:observations
weigh
1
// The syntax below allows me to use multiple lines for longer texts.
[;;;
Weighed stoichiometrically to carbonized ampoule. Barium added last to avoid
contact with ampoule during reaction]
recovered_mass: 250.0
seal
1
Evacuated ampoule and sealed with H2/O2 torch
anneal
2
[;;;
Opened under argon atmosphere and ground well before sealing in new ampoule
in between annealings.]
start_temp: 25
start_temp_unit: degree_Celsius
// Here, the double brackets signal that there are multiple program sections.
program: [[
type: ramp
temp: 600
time: 10
temp_unit: degree_Celsius
time_unit: hour
type: dwell
time: 120
time_unit: hour
]]
grind
3
dark gray powder now
recovered_mass: 200.0
[Cifs]
file_name: Ba2Zn5Sb6_ICSD
extension: .cif
embedded: {{{
#(C) 2025 by FIZ Karlsruhe - Leibniz Institute for Information Infrastructure. All rights reserved.
data_71031-ICSD
_database_code_ICSD 71031
_audit_creation_date 2023-08-01
_chemical_name_common 'Barium zinc antimonide (2/5/6)'
_chemical_formula_structural 'Ba2 Zn5 Sb6'
_chemical_formula_sum 'Ba2 Sb6 Zn5'
_exptl_crystal_density_diffrn 6.13
_diffrn_ambient_temperature 100.
_citation_title
;
New trick for an old dog: from prediction to properties of hidden clathrates
\(Ba_2 Zn_5As_6\) and \(Ba_2 Zn_5Sb_6\)
;
loop_
_citation_id
_citation_journal_full
_citation_year
_citation_journal_volume
_citation_page_first
_citation_page_last
_citation_journal_id_ASTM
primary 'Journal of the American Chemical Society' 2023 145 4638 4646 JACSAT
loop_
_citation_author_citation_id
_citation_author_name
primary 'Yox, Philip'
primary 'Cerasoli, Frank'
primary 'Sarkar, Arka'
primary 'Kyveryga, Victoria'
primary 'Viswanathan, Gayatri'
primary 'Donadio, Davide'
primary 'Kovnir, Kirill'
_cell_length_a 11.4154(5)
_cell_length_b 10.0135(4)
_cell_length_c 12.6172(5)
_cell_angle_alpha 90
_cell_angle_beta 90
_cell_angle_gamma 90
_cell_volume 1442.24
_cell_formula_units_Z 4
_space_group_name_H-M_alt 'P m n a'
_space_group_IT_number 53
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 'x+1/2, y, -z+1/2'
2 'x+1/2, -y, z+1/2'
3 '-x, y, z'
4 '-x, -y, -z'
5 '-x+1/2, -y, z+1/2'
6 '-x+1/2, y, -z+1/2'
7 'x, -y, -z'
8 'x, y, z'
loop_
_atom_type_symbol
_atom_type_oxidation_number
Ba0+ 0
Sb0+ 0
Zn0+ 0
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_symmetry_multiplicity
_atom_site_Wyckoff_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_occupancy
Ba1 Ba0+ 4 h 0.5 0.23891(4) 0.64640(3) 0.00367(9) 1
Ba2 Ba0+ 4 g 0.75 0.71608(4) 0.75 0.00794(10) 1
Sb1 Sb0+ 4 f 0.32061(4) 0.5 0.5 0.00275(10) 1
Sb2 Sb0+ 4 h 0.5 0.86799(4) 0.61427(3) 0.00219(10) 1
Sb3 Sb0+ 4 h 0.5 0.73181(4) 0.93973(3) 0.00287(10) 1
Sb4 Sb0+ 8 i 0.19164(3) 0.10079(3) 0.65092(2) 0.00228(8) 1
Sb5 Sb0+ 4 h 0.5 0.50694(4) 0.80966(3) 0.00258(10) 1
Zn1 Zn0+ 4 h 0.5 0.94723(7) 0.81658(6) 0.00330(16) 1
Zn2 Zn0+ 4 e 0.33104(7) 0. 0.5 0.00356(16) 1
Zn3 Zn0+ 4 h 0.5 0.60202(7) 0.61084(6) 0.00339(16) 1
Zn4 Zn0+ 8 i 0.15880(5) 0.65041(5) 0.41232(4) 0.00452(13) 1
loop_
_atom_site_aniso_label
_atom_site_aniso_type_symbol
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_12
_atom_site_aniso_U_13
_atom_site_aniso_U_23
Ba1 Ba0+ 0.0056(2) 0.00269(19) 0.00270(18) 0. 0. -0.00066(15)
Ba2 Ba0+ 0.0031(2) 0.0110(2) 0.0097(2) 0. -0.00029(16) 0.
Sb1 Sb0+ 0.0025(2) 0.0026(2) 0.0031(2) 0. 0. 0.00002(17)
Sb2 Sb0+ 0.0037(2) 0.0013(2) 0.0015(2) 0. 0. -0.00028(17)
Sb3 Sb0+ 0.0053(2) 0.0017(2) 0.0016(2) 0. 0. -0.00002(17)
Sb4 Sb0+ 0.00259(16) 0.00227(16) 0.00198(14) 0.00013(12) 0.00028(12)
-0.00016(12)
Sb5 Sb0+ 0.0043(2) 0.0014(2) 0.0020(2) 0. 0. 0.00017(17)
Zn1 Zn0+ 0.0041(4) 0.0027(4) 0.0032(4) 0. 0. 0.0000(3)
Zn2 Zn0+ 0.0034(4) 0.0039(4) 0.0034(4) 0. 0. -0.0007(3)
Zn3 Zn0+ 0.0043(4) 0.0023(4) 0.0036(4) 0. 0. 0.0006(3)
Zn4 Zn0+ 0.0051(3) 0.0030(3) 0.0054(3) -0.0001(2) -0.0003(2) 0.0010(2)
#End of TTdata_71031-ICSD
#################### END FOS EMBED }}}
Checkpoint 2
fos_id: TE001
fos_type: synthesis
description: My First Synthesis
group_id: kovnir-0000-0003-1152-1912
project_id: travis5672/clathrates/Ba2-TM5-Sb6
[Experimenters]
name: Travis Errthum
isu_research_group: Kovnir Group - Iowa State University
orcid: 0009-0006-1937-5672
rename: [
affiliation: isu_research_group
]
[Reaction]
nominal_formula: Ba2Zn5Sb6
nominal_amount: 250.0
nominal_amount_unit: milligram
[Products]
name: Barium Zinc Antimonide (2-5-6)
formula: Ba2Zn5Sb6
expected: True
obtained: True
expected_amount: 250.0
expected_amount_unit: milligram
obtained_amount: 200.0
obtained_amount_unit: milligram
observations: Black Powder
characterizations: PXRD, EDS, Eyeballs
structure_comments: Unique clathrate with novel polyhedra. Space group Pnma
[[Reagents]]
:name
:type
:formula
:supplier
:cas
:form
:purity
:env
:amount
:amount_unit
Barium
reagent
Ba
Thermofisher
7440-39-3
lump
0.999
Ar (g)
2.0
mol ratio
treatments: [
type: cutting
repeats: 1
observations: smaller pieces improve homogenization
]
Zinc
reagent
Zn
Sigma Aldrich
7440-66-6
powder
0.995
Ar (g)
5.0
mol ratio
Antimony
reagent
Sb
Chem Stores?
7440-36-0
powder
0.999
Ar (g)
6.0
mol ratio
[[Treatments]]
:type
:repeats
:observations
weigh
1
[;;;
Weighed stoichiometrically to carbonized ampoule. Barium added last to avoid
contact with ampoule during reaction]
recovered_mass: 250.0
seal
1
Evacuated ampoule and sealed with H2/O2 torch
anneal
2
[;;;
Opened under argon atmosphere and ground well before sealing in new ampoule
in between annealings.]
start_temp: 25
start_temp_unit: degree_Celsius
program: [[
type: ramp
temp: 600
time: 10
temp_unit: degree_Celsius
time_unit: hour
type: dwell
time: 120
time_unit: hour
]]
grind
3
dark gray powder now
recovered_mass: 200.0
// This new block has been added because I renamed a required block.
[Rename]
// Synthesis files are required to have a materials block, so
// this line specifies that it has been renamed to reagents.
materials: reagents
[Cifs]
file_name: Ba2Zn5Sb6_ICSD
extension: .cif
embedded: {{{
#(C) 2025 by FIZ Karlsruhe - Leibniz Institute for Information Infrastructure. All rights reserved.
data_71031-ICSD
_database_code_ICSD 71031
_audit_creation_date 2023-08-01
_chemical_name_common 'Barium zinc antimonide (2/5/6)'
_chemical_formula_structural 'Ba2 Zn5 Sb6'
_chemical_formula_sum 'Ba2 Sb6 Zn5'
_exptl_crystal_density_diffrn 6.13
_diffrn_ambient_temperature 100.
_citation_title
;
New trick for an old dog: from prediction to properties of hidden clathrates
\(Ba_2 Zn_5As_6\) and \(Ba_2 Zn_5Sb_6\)
;
loop_
_citation_id
_citation_journal_full
_citation_year
_citation_journal_volume
_citation_page_first
_citation_page_last
_citation_journal_id_ASTM
primary 'Journal of the American Chemical Society' 2023 145 4638 4646 JACSAT
loop_
_citation_author_citation_id
_citation_author_name
primary 'Yox, Philip'
primary 'Cerasoli, Frank'
primary 'Sarkar, Arka'
primary 'Kyveryga, Victoria'
primary 'Viswanathan, Gayatri'
primary 'Donadio, Davide'
primary 'Kovnir, Kirill'
_cell_length_a 11.4154(5)
_cell_length_b 10.0135(4)
_cell_length_c 12.6172(5)
_cell_angle_alpha 90
_cell_angle_beta 90
_cell_angle_gamma 90
_cell_volume 1442.24
_cell_formula_units_Z 4
_space_group_name_H-M_alt 'P m n a'
_space_group_IT_number 53
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 'x+1/2, y, -z+1/2'
2 'x+1/2, -y, z+1/2'
3 '-x, y, z'
4 '-x, -y, -z'
5 '-x+1/2, -y, z+1/2'
6 '-x+1/2, y, -z+1/2'
7 'x, -y, -z'
8 'x, y, z'
loop_
_atom_type_symbol
_atom_type_oxidation_number
Ba0+ 0
Sb0+ 0
Zn0+ 0
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_symmetry_multiplicity
_atom_site_Wyckoff_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_occupancy
Ba1 Ba0+ 4 h 0.5 0.23891(4) 0.64640(3) 0.00367(9) 1
Ba2 Ba0+ 4 g 0.75 0.71608(4) 0.75 0.00794(10) 1
Sb1 Sb0+ 4 f 0.32061(4) 0.5 0.5 0.00275(10) 1
Sb2 Sb0+ 4 h 0.5 0.86799(4) 0.61427(3) 0.00219(10) 1
Sb3 Sb0+ 4 h 0.5 0.73181(4) 0.93973(3) 0.00287(10) 1
Sb4 Sb0+ 8 i 0.19164(3) 0.10079(3) 0.65092(2) 0.00228(8) 1
Sb5 Sb0+ 4 h 0.5 0.50694(4) 0.80966(3) 0.00258(10) 1
Zn1 Zn0+ 4 h 0.5 0.94723(7) 0.81658(6) 0.00330(16) 1
Zn2 Zn0+ 4 e 0.33104(7) 0. 0.5 0.00356(16) 1
Zn3 Zn0+ 4 h 0.5 0.60202(7) 0.61084(6) 0.00339(16) 1
Zn4 Zn0+ 8 i 0.15880(5) 0.65041(5) 0.41232(4) 0.00452(13) 1
loop_
_atom_site_aniso_label
_atom_site_aniso_type_symbol
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_12
_atom_site_aniso_U_13
_atom_site_aniso_U_23
Ba1 Ba0+ 0.0056(2) 0.00269(19) 0.00270(18) 0. 0. -0.00066(15)
Ba2 Ba0+ 0.0031(2) 0.0110(2) 0.0097(2) 0. -0.00029(16) 0.
Sb1 Sb0+ 0.0025(2) 0.0026(2) 0.0031(2) 0. 0. 0.00002(17)
Sb2 Sb0+ 0.0037(2) 0.0013(2) 0.0015(2) 0. 0. -0.00028(17)
Sb3 Sb0+ 0.0053(2) 0.0017(2) 0.0016(2) 0. 0. -0.00002(17)
Sb4 Sb0+ 0.00259(16) 0.00227(16) 0.00198(14) 0.00013(12) 0.00028(12)
-0.00016(12)
Sb5 Sb0+ 0.0043(2) 0.0014(2) 0.0020(2) 0. 0. 0.00017(17)
Zn1 Zn0+ 0.0041(4) 0.0027(4) 0.0032(4) 0. 0. 0.0000(3)
Zn2 Zn0+ 0.0034(4) 0.0039(4) 0.0034(4) 0. 0. -0.0007(3)
Zn3 Zn0+ 0.0043(4) 0.0023(4) 0.0036(4) 0. 0. 0.0006(3)
Zn4 Zn0+ 0.0051(3) 0.0030(3) 0.0054(3) -0.0001(2) -0.0003(2) 0.0010(2)
#End of TTdata_71031-ICSD
#################### END FOS EMBED }}}
Checkpoint 3
fos_id: TE002
fos_type: synthesis
description: My Second Synthesis
group_id: kovnir-0000-0003-1152-1912
project_id: travis5672/clathrates/As28+d
[Experimenters]
name: Travis Errthum
isu_research_group: Kovnir Group - Iowa State University
orcid: 0009-0006-1937-5672
rename: [
affiliation: isu_research_group
]
[Reaction]
nominal_formula: Ba8Cu13Zn11As28.5
nominal_amount: 250.0
nominal_amount_unit: milligram
[Products]
name: Barium transition-metal arsenide (8-24-28.5)
formula: Ba8Cu13Zn11As28.5
expected: True
obtained: True
expected_amount: 250.0
expected_amount_unit: milligram
obtained_amount: 150.0
obtained_amount_unit: milligram
observations: Gray Powder
characterizations: PXRD
structure_comments: [;;;
Unique clathrate with variable occupancy on hyper-coordinate Arsenic site. Space
group Cmcm]
[[Reagents]]
:name
:type
:formula
:supplier
:cas
:form
:purity
:env
:amount
:amount_unit
Barium
reagent
Ba
Thermofisher
7440-39-3
lump
0.999
Ar (g)
2.0
mol ratio
treatments: [
type: cutting
repeats: 1
observations: smaller pieces improve homogenization
]
Zinc
reagent
Zn
Sigma Aldrich
7440-66-6
powder
0.995
Ar (g)
5.0
mol ratio
Antimony
reagent
Sb
Chem Stores?
7440-36-0
powder
0.999
Ar (g)
6.0
mol ratio
[[Treatments]]
:type
:repeats
:observations
weigh
1
[;;;
Weighed stoichiometrically to carbonized ampoule. Barium added last to avoid
contact with ampoule during reaction]
recovered_mass: 250.0
seal
1
Evacuated ampoule and sealed with H2/O2 torch
anneal
2
[;;;
Opened under argon atmosphere and ground well before sealing in new ampoule
in between annealings.]
start_temp: 25
start_temp_unit: degree_Celsius
program: [[
type: ramp
temp: 600
time: 10
temp_unit: degree_Celsius
time_unit: hour
type: dwell
time: 120
time_unit: hour
]]
grind
3
dark gray powder now
recovered_mass: 200.0
// This new block has been added because I renamed a required block.
[Rename]
// Synthesis files are required to have a materials block, so
// this line specifies that it has been renamed to reagents.
materials: reagents
[Cifs]
file_name: Ba2Zn5Sb6_ICSD
extension: .cif
embedded: {{{
#(C) 2025 by FIZ Karlsruhe - Leibniz Institute for Information Infrastructure. All rights reserved.
data_71031-ICSD
_database_code_ICSD 71031
_audit_creation_date 2023-08-01
_chemical_name_common 'Barium zinc antimonide (2/5/6)'
_chemical_formula_structural 'Ba2 Zn5 Sb6'
_chemical_formula_sum 'Ba2 Sb6 Zn5'
_exptl_crystal_density_diffrn 6.13
_diffrn_ambient_temperature 100.
_citation_title
;
New trick for an old dog: from prediction to properties of hidden clathrates
\(Ba_2 Zn_5As_6\) and \(Ba_2 Zn_5Sb_6\)
;
loop_
_citation_id
_citation_journal_full
_citation_year
_citation_journal_volume
_citation_page_first
_citation_page_last
_citation_journal_id_ASTM
primary 'Journal of the American Chemical Society' 2023 145 4638 4646 JACSAT
loop_
_citation_author_citation_id
_citation_author_name
primary 'Yox, Philip'
primary 'Cerasoli, Frank'
primary 'Sarkar, Arka'
primary 'Kyveryga, Victoria'
primary 'Viswanathan, Gayatri'
primary 'Donadio, Davide'
primary 'Kovnir, Kirill'
_cell_length_a 11.4154(5)
_cell_length_b 10.0135(4)
_cell_length_c 12.6172(5)
_cell_angle_alpha 90
_cell_angle_beta 90
_cell_angle_gamma 90
_cell_volume 1442.24
_cell_formula_units_Z 4
_space_group_name_H-M_alt 'P m n a'
_space_group_IT_number 53
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 'x+1/2, y, -z+1/2'
2 'x+1/2, -y, z+1/2'
3 '-x, y, z'
4 '-x, -y, -z'
5 '-x+1/2, -y, z+1/2'
6 '-x+1/2, y, -z+1/2'
7 'x, -y, -z'
8 'x, y, z'
loop_
_atom_type_symbol
_atom_type_oxidation_number
Ba0+ 0
Sb0+ 0
Zn0+ 0
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_symmetry_multiplicity
_atom_site_Wyckoff_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_occupancy
Ba1 Ba0+ 4 h 0.5 0.23891(4) 0.64640(3) 0.00367(9) 1
Ba2 Ba0+ 4 g 0.75 0.71608(4) 0.75 0.00794(10) 1
Sb1 Sb0+ 4 f 0.32061(4) 0.5 0.5 0.00275(10) 1
Sb2 Sb0+ 4 h 0.5 0.86799(4) 0.61427(3) 0.00219(10) 1
Sb3 Sb0+ 4 h 0.5 0.73181(4) 0.93973(3) 0.00287(10) 1
Sb4 Sb0+ 8 i 0.19164(3) 0.10079(3) 0.65092(2) 0.00228(8) 1
Sb5 Sb0+ 4 h 0.5 0.50694(4) 0.80966(3) 0.00258(10) 1
Zn1 Zn0+ 4 h 0.5 0.94723(7) 0.81658(6) 0.00330(16) 1
Zn2 Zn0+ 4 e 0.33104(7) 0. 0.5 0.00356(16) 1
Zn3 Zn0+ 4 h 0.5 0.60202(7) 0.61084(6) 0.00339(16) 1
Zn4 Zn0+ 8 i 0.15880(5) 0.65041(5) 0.41232(4) 0.00452(13) 1
loop_
_atom_site_aniso_label
_atom_site_aniso_type_symbol
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_12
_atom_site_aniso_U_13
_atom_site_aniso_U_23
Ba1 Ba0+ 0.0056(2) 0.00269(19) 0.00270(18) 0. 0. -0.00066(15)
Ba2 Ba0+ 0.0031(2) 0.0110(2) 0.0097(2) 0. -0.00029(16) 0.
Sb1 Sb0+ 0.0025(2) 0.0026(2) 0.0031(2) 0. 0. 0.00002(17)
Sb2 Sb0+ 0.0037(2) 0.0013(2) 0.0015(2) 0. 0. -0.00028(17)
Sb3 Sb0+ 0.0053(2) 0.0017(2) 0.0016(2) 0. 0. -0.00002(17)
Sb4 Sb0+ 0.00259(16) 0.00227(16) 0.00198(14) 0.00013(12) 0.00028(12)
-0.00016(12)
Sb5 Sb0+ 0.0043(2) 0.0014(2) 0.0020(2) 0. 0. 0.00017(17)
Zn1 Zn0+ 0.0041(4) 0.0027(4) 0.0032(4) 0. 0. 0.0000(3)
Zn2 Zn0+ 0.0034(4) 0.0039(4) 0.0034(4) 0. 0. -0.0007(3)
Zn3 Zn0+ 0.0043(4) 0.0023(4) 0.0036(4) 0. 0. 0.0006(3)
Zn4 Zn0+ 0.0051(3) 0.0030(3) 0.0054(3) -0.0001(2) -0.0003(2) 0.0010(2)
#End of TTdata_71031-ICSD
#################### END FOS EMBED }}}
Checkpoint 4
fos_id: TE002
fos_type: synthesis
description: My Second Synthesis
group_id: kovnir-0000-0003-1152-1912
project_id: travis5672/clathrates/As28+d
// Note that now there are two experimenters, so the
// experimenters header has changed to double brackets
[[Experimenters]]
name: Travis Errthum
isu_research_group: Kovnir Group - Iowa State University
orcid: 0009-0006-1937-5672
rename: [
affiliation: isu_research_group
]
name: Joseph Race
affiliation: Kovnir Group - Iowa State University
orcid: 0000-0002-8551-3627
[Reaction]
nominal_formula: Ba8Cu13Zn11As28.5
nominal_amount: 250.0
nominal_amount_unit: milligram
[Products]
name: Barium transition-metal arsenide (8-24-28.5)
formula: Ba8Cu13Zn11As28.5
expected: True
obtained: True
expected_amount: 250.0
expected_amount_unit: milligram
obtained_amount: 150.0
obtained_amount_unit: milligram
observations: Gray Powder
characterizations: PXRD
structure_comments: [;;;
Unique clathrate with variable occupancy on hyper-coordinate Arsenic site. Space
group Cmcm]
[[Reagents]]
:name
:type
:formula
:supplier
:cas
:form
:purity
:env
:amount
:amount_unit
Barium
reagent
Ba
Thermofisher
7440-39-3
lump
0.999
Ar (g)
2.0
mol ratio
treatments: [
type: cutting
repeats: 1
observations: smaller pieces improve homogenization
]
Zinc
reagent
Zn
Sigma Aldrich
7440-66-6
powder
0.995
Ar (g)
5.0
mol ratio
Antimony
reagent
Sb
Chem Stores?
7440-36-0
powder
0.999
Ar (g)
6.0
mol ratio
[[Treatments]]
:type
:repeats
:observations
weigh
1
[;;;
Weighed stoichiometrically to carbonized ampoule. Barium added last to avoid
contact with ampoule during reaction]
recovered_mass: 250.0
seal
1
Evacuated ampoule and sealed with H2/O2 torch
anneal
2
[;;;
Opened under argon atmosphere and ground well before sealing in new ampoule
in between annealings.]
start_temp: 25
start_temp_unit: degree_Celsius
program: [[
type: ramp
temp: 600
time: 10
temp_unit: degree_Celsius
time_unit: hour
type: dwell
time: 120
time_unit: hour
]]
grind
3
dark gray powder now
recovered_mass: 200.0
[Rename]
materials: reagents
[Cifs]
file_name: Ba2Zn5Sb6_ICSD
extension: .cif
embedded: {{{
#(C) 2025 by FIZ Karlsruhe - Leibniz Institute for Information Infrastructure. All rights reserved.
data_71031-ICSD
_database_code_ICSD 71031
_audit_creation_date 2023-08-01
_chemical_name_common 'Barium zinc antimonide (2/5/6)'
_chemical_formula_structural 'Ba2 Zn5 Sb6'
_chemical_formula_sum 'Ba2 Sb6 Zn5'
_exptl_crystal_density_diffrn 6.13
_diffrn_ambient_temperature 100.
_citation_title
;
New trick for an old dog: from prediction to properties of hidden clathrates
\(Ba_2 Zn_5As_6\) and \(Ba_2 Zn_5Sb_6\)
;
loop_
_citation_id
_citation_journal_full
_citation_year
_citation_journal_volume
_citation_page_first
_citation_page_last
_citation_journal_id_ASTM
primary 'Journal of the American Chemical Society' 2023 145 4638 4646 JACSAT
loop_
_citation_author_citation_id
_citation_author_name
primary 'Yox, Philip'
primary 'Cerasoli, Frank'
primary 'Sarkar, Arka'
primary 'Kyveryga, Victoria'
primary 'Viswanathan, Gayatri'
primary 'Donadio, Davide'
primary 'Kovnir, Kirill'
_cell_length_a 11.4154(5)
_cell_length_b 10.0135(4)
_cell_length_c 12.6172(5)
_cell_angle_alpha 90
_cell_angle_beta 90
_cell_angle_gamma 90
_cell_volume 1442.24
_cell_formula_units_Z 4
_space_group_name_H-M_alt 'P m n a'
_space_group_IT_number 53
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 'x+1/2, y, -z+1/2'
2 'x+1/2, -y, z+1/2'
3 '-x, y, z'
4 '-x, -y, -z'
5 '-x+1/2, -y, z+1/2'
6 '-x+1/2, y, -z+1/2'
7 'x, -y, -z'
8 'x, y, z'
loop_
_atom_type_symbol
_atom_type_oxidation_number
Ba0+ 0
Sb0+ 0
Zn0+ 0
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_symmetry_multiplicity
_atom_site_Wyckoff_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_occupancy
Ba1 Ba0+ 4 h 0.5 0.23891(4) 0.64640(3) 0.00367(9) 1
Ba2 Ba0+ 4 g 0.75 0.71608(4) 0.75 0.00794(10) 1
Sb1 Sb0+ 4 f 0.32061(4) 0.5 0.5 0.00275(10) 1
Sb2 Sb0+ 4 h 0.5 0.86799(4) 0.61427(3) 0.00219(10) 1
Sb3 Sb0+ 4 h 0.5 0.73181(4) 0.93973(3) 0.00287(10) 1
Sb4 Sb0+ 8 i 0.19164(3) 0.10079(3) 0.65092(2) 0.00228(8) 1
Sb5 Sb0+ 4 h 0.5 0.50694(4) 0.80966(3) 0.00258(10) 1
Zn1 Zn0+ 4 h 0.5 0.94723(7) 0.81658(6) 0.00330(16) 1
Zn2 Zn0+ 4 e 0.33104(7) 0. 0.5 0.00356(16) 1
Zn3 Zn0+ 4 h 0.5 0.60202(7) 0.61084(6) 0.00339(16) 1
Zn4 Zn0+ 8 i 0.15880(5) 0.65041(5) 0.41232(4) 0.00452(13) 1
loop_
_atom_site_aniso_label
_atom_site_aniso_type_symbol
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_12
_atom_site_aniso_U_13
_atom_site_aniso_U_23
Ba1 Ba0+ 0.0056(2) 0.00269(19) 0.00270(18) 0. 0. -0.00066(15)
Ba2 Ba0+ 0.0031(2) 0.0110(2) 0.0097(2) 0. -0.00029(16) 0.
Sb1 Sb0+ 0.0025(2) 0.0026(2) 0.0031(2) 0. 0. 0.00002(17)
Sb2 Sb0+ 0.0037(2) 0.0013(2) 0.0015(2) 0. 0. -0.00028(17)
Sb3 Sb0+ 0.0053(2) 0.0017(2) 0.0016(2) 0. 0. -0.00002(17)
Sb4 Sb0+ 0.00259(16) 0.00227(16) 0.00198(14) 0.00013(12) 0.00028(12)
-0.00016(12)
Sb5 Sb0+ 0.0043(2) 0.0014(2) 0.0020(2) 0. 0. 0.00017(17)
Zn1 Zn0+ 0.0041(4) 0.0027(4) 0.0032(4) 0. 0. 0.0000(3)
Zn2 Zn0+ 0.0034(4) 0.0039(4) 0.0034(4) 0. 0. -0.0007(3)
Zn3 Zn0+ 0.0043(4) 0.0023(4) 0.0036(4) 0. 0. 0.0006(3)
Zn4 Zn0+ 0.0051(3) 0.0030(3) 0.0054(3) -0.0001(2) -0.0003(2) 0.0010(2)
#End of TTdata_71031-ICSD
#################### END FOS EMBED }}}
Checkpoint 5
fos_id: TE002
fos_type: synthesis
description: My Second Synthesis
group_id: kovnir-0000-0003-1152-1912
project_id: travis5672/clathrates/As28+d
// Note that there are now multiple experimenters in this block,
// So the header now has double brackets
[[Experimenters]]
name: Travis Errthum
isu_research_group: Kovnir Group - Iowa State University
orcid: 0009-0006-1937-5672
rename: [
affiliation: isu_research_group
]
// This copy of Joe has information about him as Travis's colleague
colleague$experimenter: [
name: Joseph Race
affiliation: Graham's Dad
orcid: 0000-0002-8551-3627
]
// This copy of Joe has information about him as an experimenter
name: Joseph Race
affiliation: Kovnir Group - Iowa State University
orcid: 0000-0002-8551-3627
[Reaction]
nominal_formula: Ba8Cu13Zn11As28.5
nominal_amount: 250.0
nominal_amount_unit: milligram
[Products]
name: Barium transition-metal arsenide (8-24-28.5)
formula: Ba8Cu13Zn11As28.5
expected: True
obtained: True
expected_amount: 250.0
expected_amount_unit: milligram
obtained_amount: 150.0
obtained_amount_unit: milligram
observations: Gray Powder
characterizations: PXRD
structure_comments: [;;;
Unique clathrate with variable occupancy on hyper-coordinate Arsenic site. Space
group Cmcm]
[[Reagents]]
:name
:type
:formula
:supplier
:cas
:form
:purity
:env
:amount
:amount_unit
Barium
reagent
Ba
Thermofisher
7440-39-3
lump
0.999
Ar (g)
2.0
mol ratio
treatments: [
type: cutting
repeats: 1
observations: smaller pieces improve homogenization
]
Zinc
reagent
Zn
Sigma Aldrich
7440-66-6
powder
0.995
Ar (g)
5.0
mol ratio
Antimony
reagent
Sb
Chem Stores?
7440-36-0
powder
0.999
Ar (g)
6.0
mol ratio
[[Treatments]]
:type
:repeats
:observations
weigh
1
[;;;
Weighed stoichiometrically to carbonized ampoule. Barium added last to avoid
contact with ampoule during reaction]
recovered_mass: 250.0
seal
1
Evacuated ampoule and sealed with H2/O2 torch
anneal
2
[;;;
Opened under argon atmosphere and ground well before sealing in new ampoule
in between annealings.]
start_temp: 25
start_temp_unit: degree_Celsius
program: [[
type: ramp
temp: 600
time: 10
temp_unit: degree_Celsius
time_unit: hour
type: dwell
time: 120
time_unit: hour
]]
grind
3
dark gray powder now
recovered_mass: 200.0
[Rename]
materials: reagents
[Cifs]
file_name: Ba2Zn5Sb6_ICSD
extension: .cif
embedded: {{{
#(C) 2025 by FIZ Karlsruhe - Leibniz Institute for Information Infrastructure. All rights reserved.
data_71031-ICSD
_database_code_ICSD 71031
_audit_creation_date 2023-08-01
_chemical_name_common 'Barium zinc antimonide (2/5/6)'
_chemical_formula_structural 'Ba2 Zn5 Sb6'
_chemical_formula_sum 'Ba2 Sb6 Zn5'
_exptl_crystal_density_diffrn 6.13
_diffrn_ambient_temperature 100.
_citation_title
;
New trick for an old dog: from prediction to properties of hidden clathrates
\(Ba_2 Zn_5As_6\) and \(Ba_2 Zn_5Sb_6\)
;
loop_
_citation_id
_citation_journal_full
_citation_year
_citation_journal_volume
_citation_page_first
_citation_page_last
_citation_journal_id_ASTM
primary 'Journal of the American Chemical Society' 2023 145 4638 4646 JACSAT
loop_
_citation_author_citation_id
_citation_author_name
primary 'Yox, Philip'
primary 'Cerasoli, Frank'
primary 'Sarkar, Arka'
primary 'Kyveryga, Victoria'
primary 'Viswanathan, Gayatri'
primary 'Donadio, Davide'
primary 'Kovnir, Kirill'
_cell_length_a 11.4154(5)
_cell_length_b 10.0135(4)
_cell_length_c 12.6172(5)
_cell_angle_alpha 90
_cell_angle_beta 90
_cell_angle_gamma 90
_cell_volume 1442.24
_cell_formula_units_Z 4
_space_group_name_H-M_alt 'P m n a'
_space_group_IT_number 53
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 'x+1/2, y, -z+1/2'
2 'x+1/2, -y, z+1/2'
3 '-x, y, z'
4 '-x, -y, -z'
5 '-x+1/2, -y, z+1/2'
6 '-x+1/2, y, -z+1/2'
7 'x, -y, -z'
8 'x, y, z'
loop_
_atom_type_symbol
_atom_type_oxidation_number
Ba0+ 0
Sb0+ 0
Zn0+ 0
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_symmetry_multiplicity
_atom_site_Wyckoff_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_occupancy
Ba1 Ba0+ 4 h 0.5 0.23891(4) 0.64640(3) 0.00367(9) 1
Ba2 Ba0+ 4 g 0.75 0.71608(4) 0.75 0.00794(10) 1
Sb1 Sb0+ 4 f 0.32061(4) 0.5 0.5 0.00275(10) 1
Sb2 Sb0+ 4 h 0.5 0.86799(4) 0.61427(3) 0.00219(10) 1
Sb3 Sb0+ 4 h 0.5 0.73181(4) 0.93973(3) 0.00287(10) 1
Sb4 Sb0+ 8 i 0.19164(3) 0.10079(3) 0.65092(2) 0.00228(8) 1
Sb5 Sb0+ 4 h 0.5 0.50694(4) 0.80966(3) 0.00258(10) 1
Zn1 Zn0+ 4 h 0.5 0.94723(7) 0.81658(6) 0.00330(16) 1
Zn2 Zn0+ 4 e 0.33104(7) 0. 0.5 0.00356(16) 1
Zn3 Zn0+ 4 h 0.5 0.60202(7) 0.61084(6) 0.00339(16) 1
Zn4 Zn0+ 8 i 0.15880(5) 0.65041(5) 0.41232(4) 0.00452(13) 1
loop_
_atom_site_aniso_label
_atom_site_aniso_type_symbol
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_12
_atom_site_aniso_U_13
_atom_site_aniso_U_23
Ba1 Ba0+ 0.0056(2) 0.00269(19) 0.00270(18) 0. 0. -0.00066(15)
Ba2 Ba0+ 0.0031(2) 0.0110(2) 0.0097(2) 0. -0.00029(16) 0.
Sb1 Sb0+ 0.0025(2) 0.0026(2) 0.0031(2) 0. 0. 0.00002(17)
Sb2 Sb0+ 0.0037(2) 0.0013(2) 0.0015(2) 0. 0. -0.00028(17)
Sb3 Sb0+ 0.0053(2) 0.0017(2) 0.0016(2) 0. 0. -0.00002(17)
Sb4 Sb0+ 0.00259(16) 0.00227(16) 0.00198(14) 0.00013(12) 0.00028(12)
-0.00016(12)
Sb5 Sb0+ 0.0043(2) 0.0014(2) 0.0020(2) 0. 0. 0.00017(17)
Zn1 Zn0+ 0.0041(4) 0.0027(4) 0.0032(4) 0. 0. 0.0000(3)
Zn2 Zn0+ 0.0034(4) 0.0039(4) 0.0034(4) 0. 0. -0.0007(3)
Zn3 Zn0+ 0.0043(4) 0.0023(4) 0.0036(4) 0. 0. 0.0006(3)
Zn4 Zn0+ 0.0051(3) 0.0030(3) 0.0054(3) -0.0001(2) -0.0003(2) 0.0010(2)
#End of TTdata_71031-ICSD
#################### END FOS EMBED }}}
Checkpoint 6
fos_id: TE002
fos_type: synthesis
description: My Second Synthesis
group_id: kovnir-0000-0003-1152-1912
project_id: travis5672/clathrates/As28+d
[[Experimenters]]
name: Travis Errthum
isu_research_group: Kovnir Group - Iowa State University
orcid: 0009-0006-1937-5672
rename: [
affiliation: isu_research_group
]
colleague$experimenter: [
name: Joseph Race
affiliation: Graham's Dad
orcid: 0000-0002-8551-3627
]
name: Joseph Race
affiliation: Kovnir Group - Iowa State University
orcid: 0000-0002-8551-3627
[Reaction]
nominal_formula: Ba8Cu13Zn11As28.5
nominal_amount: 250.0
nominal_amount_unit: milligram
[Products]
name: Barium transition-metal arsenide (8-24-28.5)
formula: Ba8Cu13Zn11As28.5
expected: True
obtained: True
expected_amount: 250.0
expected_amount_unit: milligram
obtained_amount: 150.0
obtained_amount_unit: milligram
observations: Gray Powder
characterizations: PXRD
structure_comments: [;;;
Unique clathrate with variable occupancy on hyper-coordinate Arsenic site. Space
group Cmcm]
[[Reagents]]
name: Barium
type: reagent
formula: Ba
supplier: Thermofisher
cas: 7440-39-3
form: lump
purity: 0.999
env: Ar (g)
amount: 8
amount_unit: mol ratio
treatments: [
type: cutting
repeats: 1
observations: smaller pieces improve homogenization
]
name: Zinc
type: reagent
formula: Zn
supplier: Sigma Aldrich
cas: 7440-66-6
form: powder
purity: 0.995
env: Ar (g)
amount: 11
amount_unit: mol ratio
name: Copper
type: reagent
formula: Cu
supplier: Sigma Aldrich
cas: 7440-50-8
form: powder
env: Ar (g)
amount: 13
amount_unit: mol ratio
purity: 0.995
name: Arsenic
type: reagent
formula: As
supplier: Furukama
cas: 7440-38-2
form: lump
env: Ar (g)
amount: 28.5
amount_unit: mol ratio
purity: 0.9995
treatments: [
type: Grinding
repeats: 1
observations: ground lumps into powder for weighing and homogenization
]
[[Treatments]]
:type
:repeats
:observations
weigh
1
[;;;
Weighed stoichiometrically to carbonized ampoule. Barium added last to avoid
contact with ampoule during reaction]
recovered_mass: 250.0
seal
1
Evacuated ampoule and sealed with H2/O2 torch
anneal
2
[;;;
Opened under argon atmosphere and ground well before sealing in new ampoule
in between annealings.]
start_temp: 25
start_temp_unit: degree_Celsius
program: [[
type: ramp
temp: 600
time: 10
temp_unit: degree_Celsius
time_unit: hour
type: dwell
time: 120
time_unit: hour
]]
grind
3
dark gray powder now
recovered_mass: 200.0
[Rename]
materials: reagents
[Cifs]
file_name: Ba2Zn5Sb6_ICSD
extension: .cif
embedded: {{{
#(C) 2025 by FIZ Karlsruhe - Leibniz Institute for Information Infrastructure. All rights reserved.
data_71031-ICSD
_database_code_ICSD 71031
_audit_creation_date 2023-08-01
_chemical_name_common 'Barium zinc antimonide (2/5/6)'
_chemical_formula_structural 'Ba2 Zn5 Sb6'
_chemical_formula_sum 'Ba2 Sb6 Zn5'
_exptl_crystal_density_diffrn 6.13
_diffrn_ambient_temperature 100.
_citation_title
;
New trick for an old dog: from prediction to properties of hidden clathrates
\(Ba_2 Zn_5As_6\) and \(Ba_2 Zn_5Sb_6\)
;
loop_
_citation_id
_citation_journal_full
_citation_year
_citation_journal_volume
_citation_page_first
_citation_page_last
_citation_journal_id_ASTM
primary 'Journal of the American Chemical Society' 2023 145 4638 4646 JACSAT
loop_
_citation_author_citation_id
_citation_author_name
primary 'Yox, Philip'
primary 'Cerasoli, Frank'
primary 'Sarkar, Arka'
primary 'Kyveryga, Victoria'
primary 'Viswanathan, Gayatri'
primary 'Donadio, Davide'
primary 'Kovnir, Kirill'
_cell_length_a 11.4154(5)
_cell_length_b 10.0135(4)
_cell_length_c 12.6172(5)
_cell_angle_alpha 90
_cell_angle_beta 90
_cell_angle_gamma 90
_cell_volume 1442.24
_cell_formula_units_Z 4
_space_group_name_H-M_alt 'P m n a'
_space_group_IT_number 53
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 'x+1/2, y, -z+1/2'
2 'x+1/2, -y, z+1/2'
3 '-x, y, z'
4 '-x, -y, -z'
5 '-x+1/2, -y, z+1/2'
6 '-x+1/2, y, -z+1/2'
7 'x, -y, -z'
8 'x, y, z'
loop_
_atom_type_symbol
_atom_type_oxidation_number
Ba0+ 0
Sb0+ 0
Zn0+ 0
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_symmetry_multiplicity
_atom_site_Wyckoff_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_occupancy
Ba1 Ba0+ 4 h 0.5 0.23891(4) 0.64640(3) 0.00367(9) 1
Ba2 Ba0+ 4 g 0.75 0.71608(4) 0.75 0.00794(10) 1
Sb1 Sb0+ 4 f 0.32061(4) 0.5 0.5 0.00275(10) 1
Sb2 Sb0+ 4 h 0.5 0.86799(4) 0.61427(3) 0.00219(10) 1
Sb3 Sb0+ 4 h 0.5 0.73181(4) 0.93973(3) 0.00287(10) 1
Sb4 Sb0+ 8 i 0.19164(3) 0.10079(3) 0.65092(2) 0.00228(8) 1
Sb5 Sb0+ 4 h 0.5 0.50694(4) 0.80966(3) 0.00258(10) 1
Zn1 Zn0+ 4 h 0.5 0.94723(7) 0.81658(6) 0.00330(16) 1
Zn2 Zn0+ 4 e 0.33104(7) 0. 0.5 0.00356(16) 1
Zn3 Zn0+ 4 h 0.5 0.60202(7) 0.61084(6) 0.00339(16) 1
Zn4 Zn0+ 8 i 0.15880(5) 0.65041(5) 0.41232(4) 0.00452(13) 1
loop_
_atom_site_aniso_label
_atom_site_aniso_type_symbol
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_12
_atom_site_aniso_U_13
_atom_site_aniso_U_23
Ba1 Ba0+ 0.0056(2) 0.00269(19) 0.00270(18) 0. 0. -0.00066(15)
Ba2 Ba0+ 0.0031(2) 0.0110(2) 0.0097(2) 0. -0.00029(16) 0.
Sb1 Sb0+ 0.0025(2) 0.0026(2) 0.0031(2) 0. 0. 0.00002(17)
Sb2 Sb0+ 0.0037(2) 0.0013(2) 0.0015(2) 0. 0. -0.00028(17)
Sb3 Sb0+ 0.0053(2) 0.0017(2) 0.0016(2) 0. 0. -0.00002(17)
Sb4 Sb0+ 0.00259(16) 0.00227(16) 0.00198(14) 0.00013(12) 0.00028(12)
-0.00016(12)
Sb5 Sb0+ 0.0043(2) 0.0014(2) 0.0020(2) 0. 0. 0.00017(17)
Zn1 Zn0+ 0.0041(4) 0.0027(4) 0.0032(4) 0. 0. 0.0000(3)
Zn2 Zn0+ 0.0034(4) 0.0039(4) 0.0034(4) 0. 0. -0.0007(3)
Zn3 Zn0+ 0.0043(4) 0.0023(4) 0.0036(4) 0. 0. 0.0006(3)
Zn4 Zn0+ 0.0051(3) 0.0030(3) 0.0054(3) -0.0001(2) -0.0003(2) 0.0010(2)
#End of TTdata_71031-ICSD
#################### END FOS EMBED }}}
Checkpoint 8
fos_id: TE002
fos_type: synthesis
description: My Second Synthesis
group_id: kovnir-0000-0003-1152-1912
project_id: travis5672/clathrates/As28+d
[[Experimenters]]
name: Travis Errthum
isu_research_group: Kovnir Group - Iowa State University
orcid: 0009-0006-1937-5672
rename: [
affiliation: isu_research_group
]
colleague$experimenter: [
name: Joseph Race
affiliation: Graham's Dad
orcid: 0000-0002-8551-3627
]
name: Joseph Race
affiliation: Kovnir Group - Iowa State University
orcid: 0000-0002-8551-3627
[Reaction]
nominal_formula: Ba8Cu13Zn11As28.5
nominal_amount: 250.0
nominal_amount_unit: milligram
[Products]
name: Barium transition-metal arsenide (8-24-28.5)
formula: Ba8Cu13Zn11As28.5
expected: True
obtained: True
expected_amount: 250.0
expected_amount_unit: milligram
obtained_amount: 150.0
obtained_amount_unit: milligram
observations: Gray Powder
characterizations: PXRD
structure_comments: [;;;
Unique clathrate with variable occupancy on hyper-coordinate Arsenic site. Space
group Cmcm]
[[Reagents]]
name: Barium
type: reagent
formula: Ba
supplier: Thermofisher
cas: 7440-39-3
form: lump
purity: 0.999
env: Ar (g)
amount: 8
amount_unit: mol ratio
treatments: [
type: cutting
repeats: 1
observations: smaller pieces improve homogenization
]
name: Zinc
type: reagent
formula: Zn
supplier: Sigma Aldrich
cas: 7440-66-6
form: powder
purity: 0.995
env: Ar (g)
amount: 11
amount_unit: mol ratio
name: Copper
type: reagent
formula: Cu
supplier: Sigma Aldrich
cas: 7440-50-8
form: powder
env: Ar (g)
amount: 13
amount_unit: mol ratio
purity: 0.995
name: Arsenic
type: reagent
formula: As
supplier: Furukama
cas: 7440-38-2
form: lump
env: Ar (g)
amount: 28.5
amount_unit: mol ratio
purity: 0.9995
treatments: [
type: Grinding
repeats: 1
observations: ground lumps into powder for weighing and homogenization
]
[[Treatments]]
:type
:repeats
:observations
weigh
1
[;;;
Weighed stoichiometrically to carbonized ampoule. Barium added last to avoid
contact with ampoule during reaction]
recovered_mass: 250.0
seal
1
Evacuated ampoule and sealed with H2/O2 torch
anneal
1
None
program: [[
type: ramp
temp: 550
time: 2
temp_unit: degree_Celsius
time_unit: hour
type: dwell
time: 12
time_unit: hour
type: quench
medium: water
]]
start_temp: 25
start_temp_unit: degree_Celsius
anneal
1
None
program: [[
type: ramp
temp: 650
time: 10
temp_unit: degree_Celsius
time_unit: hour
type: dwell
time: 72
time_unit: hour
]]
start_temp: 25
start_temp_unit: degree_Celsius
[Rename]
materials: reagents
[Cifs]
file_name: Ba2Zn5Sb6_ICSD
extension: .cif
embedded: {{{
#(C) 2025 by FIZ Karlsruhe - Leibniz Institute for Information Infrastructure. All rights reserved.
data_71031-ICSD
_database_code_ICSD 71031
_audit_creation_date 2023-08-01
_chemical_name_common 'Barium zinc antimonide (2/5/6)'
_chemical_formula_structural 'Ba2 Zn5 Sb6'
_chemical_formula_sum 'Ba2 Sb6 Zn5'
_exptl_crystal_density_diffrn 6.13
_diffrn_ambient_temperature 100.
_citation_title
;
New trick for an old dog: from prediction to properties of hidden clathrates
\(Ba_2 Zn_5As_6\) and \(Ba_2 Zn_5Sb_6\)
;
loop_
_citation_id
_citation_journal_full
_citation_year
_citation_journal_volume
_citation_page_first
_citation_page_last
_citation_journal_id_ASTM
primary 'Journal of the American Chemical Society' 2023 145 4638 4646 JACSAT
loop_
_citation_author_citation_id
_citation_author_name
primary 'Yox, Philip'
primary 'Cerasoli, Frank'
primary 'Sarkar, Arka'
primary 'Kyveryga, Victoria'
primary 'Viswanathan, Gayatri'
primary 'Donadio, Davide'
primary 'Kovnir, Kirill'
_cell_length_a 11.4154(5)
_cell_length_b 10.0135(4)
_cell_length_c 12.6172(5)
_cell_angle_alpha 90
_cell_angle_beta 90
_cell_angle_gamma 90
_cell_volume 1442.24
_cell_formula_units_Z 4
_space_group_name_H-M_alt 'P m n a'
_space_group_IT_number 53
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 'x+1/2, y, -z+1/2'
2 'x+1/2, -y, z+1/2'
3 '-x, y, z'
4 '-x, -y, -z'
5 '-x+1/2, -y, z+1/2'
6 '-x+1/2, y, -z+1/2'
7 'x, -y, -z'
8 'x, y, z'
loop_
_atom_type_symbol
_atom_type_oxidation_number
Ba0+ 0
Sb0+ 0
Zn0+ 0
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_symmetry_multiplicity
_atom_site_Wyckoff_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_occupancy
Ba1 Ba0+ 4 h 0.5 0.23891(4) 0.64640(3) 0.00367(9) 1
Ba2 Ba0+ 4 g 0.75 0.71608(4) 0.75 0.00794(10) 1
Sb1 Sb0+ 4 f 0.32061(4) 0.5 0.5 0.00275(10) 1
Sb2 Sb0+ 4 h 0.5 0.86799(4) 0.61427(3) 0.00219(10) 1
Sb3 Sb0+ 4 h 0.5 0.73181(4) 0.93973(3) 0.00287(10) 1
Sb4 Sb0+ 8 i 0.19164(3) 0.10079(3) 0.65092(2) 0.00228(8) 1
Sb5 Sb0+ 4 h 0.5 0.50694(4) 0.80966(3) 0.00258(10) 1
Zn1 Zn0+ 4 h 0.5 0.94723(7) 0.81658(6) 0.00330(16) 1
Zn2 Zn0+ 4 e 0.33104(7) 0. 0.5 0.00356(16) 1
Zn3 Zn0+ 4 h 0.5 0.60202(7) 0.61084(6) 0.00339(16) 1
Zn4 Zn0+ 8 i 0.15880(5) 0.65041(5) 0.41232(4) 0.00452(13) 1
loop_
_atom_site_aniso_label
_atom_site_aniso_type_symbol
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_12
_atom_site_aniso_U_13
_atom_site_aniso_U_23
Ba1 Ba0+ 0.0056(2) 0.00269(19) 0.00270(18) 0. 0. -0.00066(15)
Ba2 Ba0+ 0.0031(2) 0.0110(2) 0.0097(2) 0. -0.00029(16) 0.
Sb1 Sb0+ 0.0025(2) 0.0026(2) 0.0031(2) 0. 0. 0.00002(17)
Sb2 Sb0+ 0.0037(2) 0.0013(2) 0.0015(2) 0. 0. -0.00028(17)
Sb3 Sb0+ 0.0053(2) 0.0017(2) 0.0016(2) 0. 0. -0.00002(17)
Sb4 Sb0+ 0.00259(16) 0.00227(16) 0.00198(14) 0.00013(12) 0.00028(12)
-0.00016(12)
Sb5 Sb0+ 0.0043(2) 0.0014(2) 0.0020(2) 0. 0. 0.00017(17)
Zn1 Zn0+ 0.0041(4) 0.0027(4) 0.0032(4) 0. 0. 0.0000(3)
Zn2 Zn0+ 0.0034(4) 0.0039(4) 0.0034(4) 0. 0. -0.0007(3)
Zn3 Zn0+ 0.0043(4) 0.0023(4) 0.0036(4) 0. 0. 0.0006(3)
Zn4 Zn0+ 0.0051(3) 0.0030(3) 0.0054(3) -0.0001(2) -0.0003(2) 0.0010(2)
#End of TTdata_71031-ICSD
#################### END FOS EMBED }}}
Checkpoint 9
fos_id: TE002
fos_type: synthesis
description: My Second Synthesis
group_id: kovnir-0000-0003-1152-1912
project_id: travis5672/clathrates/As28+d
[[Experimenters]]
name: Travis Errthum
isu_research_group: Kovnir Group - Iowa State University
orcid: 0009-0006-1937-5672
rename: [
affiliation: isu_research_group
]
colleague$experimenter: [
name: Joseph Race
affiliation: Graham's Dad
orcid: 0000-0002-8551-3627
]
name: Joseph Race
affiliation: Kovnir Group - Iowa State University
orcid: 0000-0002-8551-3627
[Reaction]
nominal_formula: Ba8Cu13Zn11As28.5
nominal_amount: 250.0
nominal_amount_unit: milligram
[Products]
name: Barium transition-metal arsenide (8-24-28.5)
formula: Ba8Cu13Zn11As28.5
expected: True
obtained: True
expected_amount: 250.0
expected_amount_unit: milligram
obtained_amount: 150.0
obtained_amount_unit: milligram
observations: Gray Powder
characterizations: PXRD
structure_comments: [;;;
Unique clathrate with variable occupancy on hyper-coordinate Arsenic site. Space
group Cmcm]
[[Reagents]]
name: Barium
type: reagent
formula: Ba
supplier: Thermofisher
cas: 7440-39-3
form: lump
purity: 0.999
env: Ar (g)
amount: 8
amount_unit: mol ratio
treatments: [
type: cutting
repeats: 1
observations: smaller pieces improve homogenization
]
name: Zinc
type: reagent
formula: Zn
supplier: Sigma Aldrich
cas: 7440-66-6
form: powder
purity: 0.995
env: Ar (g)
amount: 11
amount_unit: mol ratio
name: Copper
type: reagent
formula: Cu
supplier: Sigma Aldrich
cas: 7440-50-8
form: powder
env: Ar (g)
amount: 13
amount_unit: mol ratio
purity: 0.995
name: Arsenic
type: reagent
formula: As
supplier: Furukama
cas: 7440-38-2
form: lump
env: Ar (g)
amount: 28.5
amount_unit: mol ratio
purity: 0.9995
treatments: [
type: Grinding
repeats: 1
observations: ground lumps into powder for weighing and homogenization
]
[[Treatments]]
:type
:repeats
:observations
weigh
1
[;;;
Weighed stoichiometrically to carbonized ampoule. Barium added last to avoid
contact with ampoule during reaction]
recovered_mass: 250.0
seal
1
Evacuated ampoule and sealed with H2/O2 torch
anneal
1
None
program: [[
type: ramp
temp: 550
time: 2
temp_unit: degree_Celsius
time_unit: hour
type: dwell
time: 12
time_unit: hour
type: quench
medium: water
]]
start_temp: 25
start_temp_unit: degree_Celsius
anneal
1
None
program: [[
type: ramp
temp: 650
time: 10
temp_unit: degree_Celsius
time_unit: hour
type: dwell
time: 72
time_unit: hour
]]
start_temp: 25
start_temp_unit: degree_Celsius
[Rename]
materials: reagents
[Cifs]
file_name: PY618_Ba8-Cu12-Zn12-As29,8
extension: .cif
path: ../templates
Checkpoint 10
fos_id: TE002
fos_type: synthesis
description: My Second Synthesis
group_id: kovnir-0000-0003-1152-1912
project_id: travis5672/clathrates/As28+d
[Rename]
materials: reagents
[[Experimenters]]
name: Travis Errthum
isu_research_group: Kovnir Group - Iowa State University
orcid: 0009-0006-1937-5672
rename: [
affiliation: isu_research_group
]
colleague$experimenter: [
name: Joseph Race
affiliation: Graham's Dad
orcid: 0000-0002-8551-3627
]
name: Joseph Race
affiliation: Kovnir Group - Iowa State University
orcid: 0000-0002-8551-3627
[Reaction]
nominal_formula: Ba8Cu13Zn11As28.5
nominal_amount: 250.0
nominal_amount_unit: milligram
[Products]
name: Barium transition-metal arsenide (8-24-28.5)
formula: Ba8Cu13Zn11As28.5
expected: True
obtained: True
expected_amount: 250.0
expected_amount_unit: milligram
obtained_amount: 150.0
obtained_amount_unit: milligram
observations: Gray Powder
characterizations: PXRD
structure_comments: [;;;
Unique clathrate with variable occupancy on hyper-coordinate Arsenic site. Space
group Cmcm]
[[Reagents]]
:name
:type
:formula
:supplier
:cas
:form
:purity
:env
:amount
:amount_unit
Barium
reagent
Ba
Thermofisher
7440-39-3
lump
0.999
Ar (g)
// Weight percents were calculated automatically when saving.
// ! Total weight percent: 22.99%
8
mol ratio
treatments: [
type: cutting
repeats: 1
observations: smaller pieces improve homogenization
]
Zinc
reagent
Zn
Sigma Aldrich
7440-66-6
powder
0.995
Ar (g)
// ! Total weight percent: 15.05%
11
mol ratio
Copper
reagent
Cu
Sigma Aldrich
7440-50-8
powder
0.995
Ar (g)
// ! Total weight percent: 17.29%
13
mol ratio
Arsenic
reagent
As
Furukama
7440-38-2
lump
0.9995
Ar (g)
// ! Total weight percent: 44.68%
28.5
mol ratio
treatments: [
type: Grinding
repeats: 1
observations: ground lumps into powder for weighing and homogenization
]
[[Treatments]]
:type
:repeats
:observations
weigh
1
[;;;
Weighed stoichiometrically to carbonized ampoule. Barium added last to avoid
contact with ampoule during reaction]
recovered_mass: 250.0
seal
1
Evacuated ampoule and sealed with H2/O2 torch
anneal
1
None
program: [[
type: ramp
// ! Rate for ramp: 262.5 delta_degree_Celsius / hour
temp: 550
time: 2
temp_unit: degree_Celsius
time_unit: hour
type: dwell
time: 12
time_unit: hour
type: quench
medium: water
]]
start_temp: 25
start_temp_unit: degree_Celsius
anneal
1
None
program: [[
type: ramp
// ! Rate for ramp: 62.5 delta_degree_Celsius / hour
temp: 650
time: 10
temp_unit: degree_Celsius
time_unit: hour
type: dwell
time: 72
time_unit: hour
]]
start_temp: 25
start_temp_unit: degree_Celsius
[Cifs]
file_name: PY618_Ba8-Cu12-Zn12-As29,8
extension: .cif
path: .