data_global
_journal_name_full               CrystEngComm

# Attachment '025GPa_r.cif'

_journal_coden_Cambridge         1350

_publ_section_title              
;
LOW TEMPERATURE / HIGH PRESSURE POLYMORPHISM IN DL-CYSTEINE
;

# 1. SUBMISSION DETAILS
_publ_contact_author_name        'Elena V. Boldyreva'
_publ_contact_author_address     
;Department of Solid State Chemistry,
REC-008 Molecular Design and Ecologically Safe
Technologies,
Novosibirsk State University, Pirogov St. 2,
Novosibirsk, 630090, Russian Federation
;
_publ_contact_author_email       eboldyreva@yahoo.com
_publ_contact_author_phone       (383)3634272
_publ_contact_author_fax         (383)3634132
loop_
_publ_author_name
_publ_author_address
V.S.Minkov
;Department of Solid State Chemistry,
REC-008 Molecular Design and Ecologically Safe
Technologies,
Novosibirsk State University, Pirogov St. 2,
Novosibirsk, 630090, Russian Federation
;
N.A.Tumanov
;Department of Solid State Chemistry,
REC-008 Molecular Design and Ecologically Safe
Technologies,
Novosibirsk State University, Pirogov St. 2,
Novosibirsk, 630090, Russian Federation
;
E.V.Boldyreva
;Department of Solid State Chemistry,
REC-008 Molecular Design and Ecologically Safe
Technologies,
Novosibirsk State University, Pirogov St. 2,
Novosibirsk, 630090, Russian Federation
;
'R.Quesada Cabrera'
;Swiss-Norwegian Beam line at the ESRF,
38043 Grenoble, France
;

# Attachment '085GPa_r.cif'

data_DLCYS85_publ
_database_code_depnum_ccdc_archive 'CCDC 773688'
_audit_creation_method           'from EXP file using GSAS2CIF'

# 2. SAMPLE PREPARATION DATA
_refine_ls_shift/su_max          0.02
_refine_ls_shift/su_mean         0.00
_computing_structure_refinement  GSAS
_refine_ls_number_parameters     43
_refine_ls_number_restraints     35
_refine_ls_matrix_type           full
_refine_ls_goodness_of_fit_all   0.1443 # Reduced CHI**2
_exptl_crystal_preparation       'powder sample'

# 3. CHEMICAL, STRUCTURAL AND CRYSTAL DATA
_pd_char_particle_morphology     plate
_pd_char_colour                  white
_chemical_name_common            DL-cysteine
_chemical_formula_moiety         'C3 H7 N O2 S'
_chemical_formula_sum            'C3 H7 N O2 S'
_chemical_formula_weight         121.17
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 1 21/a 1'
_symmetry_space_group_name_Hall  '-P 2yab'
_exptl_crystal_density_diffrn    1.543
_cell_formula_units_Z            4
_cell_length_a                   9.6352(4)
_cell_length_b                   4.9435(2)
_cell_length_c                   12.8853(5)
_cell_angle_alpha                90.0
_cell_angle_beta                 121.808(2)
_cell_angle_gamma                90.0
_cell_volume                     521.57(4)
_cell_measurement_temperature    293
_cell_measurement_pressure       850000 #in kPa
_exptl_special_details           
;
polymorph II at 0.85 GPa
;

loop_
_symmetry_equiv_pos_site_id
_symmetry_equiv_pos_as_xyz
1 +x,+y,+z
2 -x+1/2,+y+1/2,-z
3 -x,-y,-z
4 +x+1/2,-y+1/2,+z

# ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS

loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_thermal_displace_type
_atom_site_U_iso_or_equiv
C C1 -0.0032(6) 0.1228(7) 0.16471(33) Uiso 0.025
C C2 0.1119(5) 0.1090(8) 0.30175(31) Uiso 0.025
C C3 0.2484(5) -0.0973(11) 0.3403(7) Uiso 0.025
H H1 -0.1003(9) 0.2297(12) 0.1467(6) Uiso 0.03
H H2 0.0520(14) 0.2208(13) 0.1293(7) Uiso 0.03
H H3 0.1638(8) 0.2909(11) 0.3302(6) Uiso 0.03
H H4 0.0814(12) -0.062(11) 0.428(4) Uiso 0.03
H H5 -0.0755(26) -0.032(13) 0.309(4) Uiso 0.03
H H6 0.001(5) 0.207(7) 0.390(8) Uiso 0.03
H H7 -0.161(8) -0.2823(15) 0.121(7) Uiso 0.03
O O1 0.3553(8) -0.0312(13) 0.3163(7) Uiso 0.025
O O2 0.2548(6) -0.2936(11) 0.4027(5) Uiso 0.025
N N1 0.0209(8) 0.0496(14) 0.3629(6) Uiso 0.025
S S1 -0.0714(5) -0.2029(7) 0.0891(4) Uiso 0.025

# MOLECULAR GEOMETRY

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
C1 H2 0.991(13)
C1 H1 0.990(10)
C1 C2 1.513(5)
C2 H3 1.000(7)
C3 C2 1.526(8)
O1 C3 1.265(11)
O2 C3 1.241(8)
N1 H6 0.91(5)
N1 H4 0.91(5)
N1 H5 0.91(5)
N1 C2 1.484(10)
S1 H7 1.20(8)
S1 C1 1.816(5)

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
H7 S1 C1 103.2(17)
H6 N1 H4 109(6)
H6 N1 H5 109(6)
H6 N1 C2 109.5(33)
H4 N1 H5 110(5)
H4 N1 C2 109.5(19)
H5 N1 C2 109.4(19)
S1 C1 H2 108.48(27)
S1 C1 H1 108.5(6)
S1 C1 C2 114.93(20)
H2 C1 H1 107.6(8)
H2 C1 C2 108.58(35)
H1 C1 C2 108.54(26)
N1 C2 C1 110.7(5)
N1 C2 H3 107.8(6)
N1 C2 C3 110.12(27)
C1 C2 H3 107.7(5)
C1 C2 C3 112.67(23)
H3 C2 C3 107.6(6)
O2 C3 O1 126.3(7)
O2 C3 C2 118.3(4)
O1 C3 C2 114.9(6)

# 4. INSTRUMENT CHARACTERIZATION

_diffrn_ambient_temperature      293
_diffrn_ambient_pressure         850000 #in kPa
_diffrn_source                   synchrotron
_diffrn_source_type              'SNBL ESRF'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_wavelength     0.70007


# Attachment '025GPa_r.cif'

data_DLCYS25_publ
_database_code_depnum_ccdc_archive 'CCDC 773689'

_audit_creation_method           'from EXP file using GSAS2CIF'

# 2. SAMPLE PREPARATION DATA
_refine_ls_shift/su_max          0.05
_refine_ls_shift/su_mean         0.01
_computing_structure_refinement  GSAS
_refine_ls_number_parameters     43
_refine_ls_number_restraints     35
_refine_ls_matrix_type           full
_refine_ls_goodness_of_fit_all   0.2005 # Reduced CHI**2
_exptl_crystal_preparation       'powder sample'

# 3. CHEMICAL, STRUCTURAL AND CRYSTAL DATA
_pd_char_particle_morphology     plate
_pd_char_colour                  white
_chemical_name_common            DL-cysteine
_chemical_formula_moiety         'C3 H7 N O2 S'
_chemical_formula_sum            'C3 H7 N O2 S'
_chemical_formula_weight         121.17
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 1 21/a 1'
_symmetry_space_group_name_Hall  '-P 2yab'
_exptl_crystal_density_diffrn    1.496
_cell_formula_units_Z            4
_cell_length_a                   9.712(5)
_cell_length_b                   4.9755(20)
_cell_length_c                   13.107(6)
_cell_angle_alpha                90.0
_cell_angle_beta                 121.849(25)
_cell_angle_gamma                90.0
_cell_volume                     538.0(4)
_cell_measurement_temperature    293
_cell_measurement_pressure       250000 #in kPa
_exptl_special_details           
;
polymorph II at 0.25 GPa
;

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

# ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS

loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_thermal_displace_type
_atom_site_U_iso_or_equiv
C C1 0.0000(6) 0.1279(7) 0.17090(27) Uiso 0.025
C C2 0.1174(5) 0.1124(8) 0.30538(26) Uiso 0.025
C C3 0.2521(5) -0.0945(9) 0.3417(5) Uiso 0.025
H H1 -0.0968(8) 0.2297(10) 0.1554(5) Uiso 0.03
H H2 0.0518(11) 0.2313(12) 0.1355(4) Uiso 0.03
H H3 0.1703(8) 0.2925(9) 0.3324(4) Uiso 0.03
H H4 0.0874(21) -0.065(16) 0.428(8) Uiso 0.03
H H5 -0.0699(35) -0.005(21) 0.316(4) Uiso 0.03
H H6 0.023(8) 0.214(12) 0.402(11) Uiso 0.03
H H7 -0.187(5) -0.2411(26) 0.095(7) Uiso 0.03
O O1 0.3493(9) -0.0405(14) 0.3080(7) Uiso 0.025
O O2 0.2612(6) -0.2887(11) 0.4044(6) Uiso 0.025
N N1 0.0312(9) 0.0587(14) 0.3690(5) Uiso 0.025
S S1 -0.0666(5) -0.1933(8) 0.09373(34) Uiso 0.025

# MOLECULAR GEOMETRY

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
C1 C2 1.514(5)
C1 H1 0.990(9)
C1 H2 0.990(10)
C1 S1 1.818(5)
C2 C3 1.530(7)
C2 H3 1.000(7)
C2 N1 1.485(10)
C3 O1 1.264(11)
C3 O2 1.241(8)
N1 H4 0.91(8)
N1 H5 0.92(5)
N1 H6 0.91(8)
S1 H7 1.20(7)

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
C2 C1 H1 108.4(5)
C2 C1 H2 108.4(6)
C2 C1 S1 115.6(3)
H1 C1 H2 107.5(7)
H1 C1 S1 108.4(5)
H2 C1 S1 108.4(5)
C1 C2 C3 113.0(4)
C1 C2 H3 107.3(4)
C1 C2 N1 111.2(5)
C3 C2 H3 107.3(6)
C3 C2 N1 110.3(4)
H3 C2 N1 107.4(6)
C2 C3 O1 115.0(5)
C2 C3 O2 118.7(6)
O1 C3 O2 126.3(6)
C2 N1 H4 109.5(35)
C2 N1 H5 109.5(25)
C2 N1 H6 109(5)
H4 N1 H5 108(7)
H4 N1 H6 109(9)
H5 N1 H6 110(9)
C1 S1 H7 103.2(12)

# 4. INSTRUMENT CHARACTERIZATION

_diffrn_ambient_temperature      293
_diffrn_ambient_pressure         250000 #in kPa
_diffrn_source                   synchrotron
_diffrn_source_type              'SNBL ESRF'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_wavelength     0.70007