# Supplementary Material (ESI) for CrystEngComm
# This journal is (c) The Royal Society of Chemistry 2010

data_global
_journal_name_full               CrystEngComm

_journal_coden_Cambridge         1350

_publ_contact_author_name        'Andrzej Katrusiak'
_publ_contact_author_email       KATRAN@AMU.EDU.PL

_publ_section_title              
;
Molecular association in low-temperature and
high-pressure polymorphs of 1,1,1,2-tetrachloroethane
;
loop_
_publ_author_name
'Andrzej Katrusiak'
'Maciej Bujak'

# Attachment '1112TCE_CIF_LT_HPall16.cif'

data_1112TCE_195K
_database_code_depnum_ccdc_archive 'CCDC 746844'
#TrackingRef '1112TCE_CIF_LT_HPall16.cif'

# CHEMICAL DATA

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
1,1,1,2-tetrachloroethane
;
_chemical_name_common            1,1,1,2-tetrachloroethane
_chemical_melting_point          ?
_chemical_formula_moiety         'C2 H2 Cl4'
_chemical_formula_sum            'C2 H2 Cl4'
_chemical_formula_weight         167.84

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

# CRYSTAL DATA

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'C 2/c'
_symmetry_space_group_name_Hall  '-C 2yc'

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

_cell_length_a                   22.2760(8)
_cell_length_b                   5.59764(17)
_cell_length_c                   10.3599(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 109.912(4)
_cell_angle_gamma                90.00
_cell_volume                     1214.58(8)
_cell_formula_units_Z            8
_cell_measurement_temperature    195.0(1)
_cell_measurement_reflns_used    3399
_cell_measurement_theta_min      3.73
_cell_measurement_theta_max      26.27

_exptl_crystal_description       irregular
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.836
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             656
_exptl_absorpt_coefficient_mu    1.802
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.6139
_exptl_absorpt_correction_T_max  0.7145
_exptl_absorpt_process_details   
;
Correction for absorption was made using CrysAlisRED
(Oxford Diffraction, 2007).
;

_exptl_special_details           
;
Data were collected at ambient pressure (100 kPa) and 195 K with
the crystal obtained by the in-situ low-temperature crystallization
technique.
;

# EXPERIMENTAL DATA

_diffrn_ambient_temperature      195.0(1)
_diffrn_ambient_pressure         100
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'KM-4 CCD'
_diffrn_measurement_method       ω-scans
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        0
_diffrn_reflns_number            4591
_diffrn_reflns_av_R_equivalents  0.0200
_diffrn_reflns_av_sigmaI/netI    0.0128
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_k_min       -4
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_theta_min         3.77
_diffrn_reflns_theta_max         25.00
_reflns_number_total             1076
_reflns_number_gt                927
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'CrysAlisCCD (Oxford Diffraction, 2007)'
_computing_cell_refinement       'CrysAlisRED (Oxford Diffraction, 2007)'
_computing_data_reduction        'CrysAlisRED (Oxford Diffraction, 2007)'
_computing_structure_solution    'SHELXS--97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL--97 (Sheldrick, 1997)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 1990)'
_computing_publication_material  'SHELXL--97 (Sheldrick, 1997)'

# REFINEMENT DATA

_refine_special_details          
;
Refinement of F² against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F², conventional R-factors R are based
on F, with F set to zero for negative F². The threshold expression of
F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F² are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0340P)²+3.5032P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     SHELXL
_refine_ls_extinction_coef       0.0062(11)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         1076
_refine_ls_number_parameters     75
_refine_ls_number_restraints     12
_refine_ls_R_factor_all          0.0441
_refine_ls_R_factor_gt           0.0383
_refine_ls_wR_factor_ref         0.0940
_refine_ls_wR_factor_gt          0.0898
_refine_ls_goodness_of_fit_ref   1.104
_refine_ls_restrained_S_all      1.553
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

# ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Cl1 Cl 0.69355(6) -0.0148(2) 0.49137(13) 0.0596(5) Uani 1 1 d . . .
Cl2 Cl 0.68800(7) 0.3780(2) 0.68212(14) 0.0653(5) Uani 1 1 d U . .
Cl3 Cl 0.59541(10) 0.3684(3) 0.40967(15) 0.0936(7) Uani 1 1 d . . .
Cl4 Cl 0.54923(7) 0.2019(3) 0.65110(17) 0.0874(6) Uani 1 1 d U . .
C11 C 0.6441(5) 0.1851(13) 0.5469(7) 0.042(2) Uani 0.69(2) 1 d P A 1
C21 C 0.6014(4) 0.0270(15) 0.5978(8) 0.050(3) Uani 0.69(2) 1 d P A 1
H211 H 0.6275 -0.0700 0.6738 0.060 Uiso 0.69(2) 1 calc PR A 1
H212 H 0.5771 -0.0793 0.5247 0.060 Uiso 0.69(2) 1 calc PR A 1
C12 C 0.6151(11) 0.229(4) 0.5741(17) 0.045(6) Uani 0.31(2) 1 d P A 2
C22 C 0.6331(10) -0.017(3) 0.5621(18) 0.049(7) Uani 0.31(2) 1 d P A 2
H221 H 0.5967 -0.1058 0.5036 0.059 Uiso 0.31(2) 1 calc PR A 2
H222 H 0.6481 -0.0918 0.6518 0.059 Uiso 0.31(2) 1 calc PR A 2

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Cl1 0.0575(8) 0.0680(8) 0.0592(8) -0.0038(6) 0.0275(6) 0.0087(6)
Cl2 0.0713(8) 0.0612(8) 0.0576(8) -0.0106(6) 0.0142(6) -0.0235(6)
Cl3 0.1402(16) 0.0719(10) 0.0473(8) 0.0146(7) 0.0039(8) 0.0333(10)
Cl4 0.0526(8) 0.1299(14) 0.0869(10) -0.0522(10) 0.0329(7) -0.0126(8)
C11 0.044(5) 0.044(4) 0.037(4) 0.003(3) 0.013(3) 0.002(3)
C21 0.043(5) 0.063(5) 0.048(4) -0.013(3) 0.021(3) -0.013(3)
C12 0.038(10) 0.053(11) 0.035(8) -0.001(7) 0.002(7) -0.006(8)
C22 0.050(12) 0.051(10) 0.046(9) -0.004(7) 0.015(8) -0.010(8)

# MOLECULAR GEOMETRY

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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cl1 C11 1.797(11) . ?
Cl1 C22 1.74(3) . ?
Cl2 C11 1.776(7) . ?
Cl2 C12 1.830(15) . ?
Cl3 C11 1.788(7) . ?
Cl3 C12 1.787(16) . ?
Cl4 C12 1.90(3) . ?
Cl4 C21 1.747(11) . ?
C11 C21 1.519(16) . ?
C12 C22 1.45(4) . ?
C21 H211 0.9700 . ?
C21 H212 0.9700 . ?
C22 H221 0.9700 . ?
C22 H222 0.9700 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C21 C11 Cl2 108.8(7) . . ?
C21 C11 Cl3 109.2(7) . . ?
Cl2 C11 Cl3 107.5(4) . . ?
C21 C11 Cl1 105.8(6) . . ?
Cl2 C11 Cl1 113.4(5) . . ?
Cl3 C11 Cl1 112.0(5) . . ?
C11 C21 Cl4 110.2(7) . . ?
C11 C21 H211 109.6 . . ?
Cl4 C21 H211 109.6 . . ?
C11 C21 H212 109.6 . . ?
Cl4 C21 H212 109.6 . . ?
H211 C21 H212 108.1 . . ?
C22 C12 Cl3 108.5(18) . . ?
C22 C12 Cl2 105.7(17) . . ?
Cl3 C12 Cl2 105.2(9) . . ?
C22 C12 Cl4 103.7(15) . . ?
Cl3 C12 Cl4 117.5(12) . . ?
Cl2 C12 Cl4 115.6(12) . . ?
C12 C22 Cl1 108.0(17) . . ?
C12 C22 H221 110.1 . . ?
Cl1 C22 H221 110.1 . . ?
C12 C22 H222 110.1 . . ?
Cl1 C22 H222 110.1 . . ?
H221 C22 H222 108.4 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Cl2 C11 C21 Cl4 59.2(7) . . . . ?
Cl3 C11 C21 Cl4 -57.8(7) . . . . ?
Cl1 C11 C21 Cl4 -178.5(3) . . . . ?
Cl3 C12 C22 Cl1 54.1(15) . . . . ?
Cl2 C12 C22 Cl1 -58.3(14) . . . . ?
Cl4 C12 C22 Cl1 179.8(7) . . . . ?

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         0.578
_refine_diff_density_min         -0.362
_refine_diff_density_rms         0.060

#############################################################################

data_1112TCE_100K
_database_code_depnum_ccdc_archive 'CCDC 746845'
#TrackingRef '1112TCE_CIF_LT_HPall16.cif'

# CHEMICAL DATA

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
1,1,1,2-tetrachloroethane
;
_chemical_name_common            1,1,1,2-tetrachloroethane
_chemical_melting_point          ?
_chemical_formula_moiety         'C2 H2 Cl4'
_chemical_formula_sum            'C2 H2 Cl4'
_chemical_formula_weight         167.84

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

# CRYSTAL DATA

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'C 2/c'
_symmetry_space_group_name_Hall  '-C 2yc'

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

_cell_length_a                   22.1891(15)
_cell_length_b                   5.4975(2)
_cell_length_c                   10.2493(6)
_cell_angle_alpha                90.00
_cell_angle_beta                 110.055(7)
_cell_angle_gamma                90.00
_cell_volume                     1174.45(12)
_cell_formula_units_Z            8
_cell_measurement_temperature    100.0(1)
_cell_measurement_reflns_used    3882
_cell_measurement_theta_min      3.75
_cell_measurement_theta_max      30.04

_exptl_crystal_description       irregular
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.898
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             656
_exptl_absorpt_coefficient_mu    1.864
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.6048
_exptl_absorpt_correction_T_max  0.7069
_exptl_absorpt_process_details   
;
Correction for absorption was made using CrysAlisRED
(Oxford Diffraction, 2007).
;

_exptl_special_details           
;
Data were collected at ambient pressure (100 kPa) and 100 K with
the crystal obtained by the in-situ low-temperature crystallization
technique.
;

# EXPERIMENTAL DATA

_diffrn_ambient_temperature      100.0(1)
_diffrn_ambient_pressure         100
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'KM-4 CCD'
_diffrn_measurement_method       ω-scans
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        0
_diffrn_reflns_number            4398
_diffrn_reflns_av_R_equivalents  0.0172
_diffrn_reflns_av_sigmaI/netI    0.0117
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_k_min       -4
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_theta_min         3.83
_diffrn_reflns_theta_max         25.00
_reflns_number_total             1034
_reflns_number_gt                944
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'CrysAlisCCD (Oxford Diffraction, 2007)'
_computing_cell_refinement       'CrysAlisRED (Oxford Diffraction, 2007)'
_computing_data_reduction        'CrysAlisRED (Oxford Diffraction, 2007)'
_computing_structure_solution    'SHELXS--97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL--97 (Sheldrick, 1997)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 1990)'
_computing_publication_material  'SHELXL--97 (Sheldrick, 1997)'

# REFINEMENT DATA

_refine_special_details          
;
Refinement of F² against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F², conventional R-factors R are based
on F, with F set to zero for negative F². The threshold expression of
F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F² are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0089P)²+3.8001P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     SHELXL
_refine_ls_extinction_coef       0.0013(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         1034
_refine_ls_number_parameters     75
_refine_ls_number_restraints     12
_refine_ls_R_factor_all          0.0294
_refine_ls_R_factor_gt           0.0261
_refine_ls_wR_factor_ref         0.0543
_refine_ls_wR_factor_gt          0.0523
_refine_ls_goodness_of_fit_ref   1.084
_refine_ls_restrained_S_all      1.317
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

# ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Cl1 Cl 0.69409(3) -0.01567(14) 0.48899(7) 0.0329(2) Uani 1 1 d . . .
Cl2 Cl 0.68902(4) 0.37962(15) 0.68299(8) 0.0413(2) Uani 1 1 d U . .
Cl3 Cl 0.59493(5) 0.37070(17) 0.40782(8) 0.0591(3) Uani 1 1 d . . .
Cl4 Cl 0.54904(4) 0.19685(19) 0.65215(9) 0.0524(3) Uani 1 1 d U . .
C11 C 0.6446(3) 0.1843(8) 0.5459(4) 0.0226(15) Uani 0.702(15) 1 d P A 1
C21 C 0.6018(3) 0.0208(9) 0.5973(5) 0.0291(15) Uani 0.702(15) 1 d P A 1
H211 H 0.6282 -0.0783 0.6739 0.035 Uiso 0.702(15) 1 calc PR A 1
H212 H 0.5774 -0.0871 0.5231 0.035 Uiso 0.702(15) 1 calc PR A 1
C12 C 0.6144(7) 0.227(2) 0.5746(11) 0.032(4) Uani 0.298(15) 1 d P A 2
C22 C 0.6325(7) -0.018(2) 0.5618(12) 0.034(4) Uani 0.298(15) 1 d P A 2
H221 H 0.5958 -0.1086 0.5024 0.041 Uiso 0.298(15) 1 calc PR A 2
H222 H 0.6476 -0.0952 0.6523 0.041 Uiso 0.298(15) 1 calc PR A 2

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Cl1 0.0323(4) 0.0380(4) 0.0305(4) -0.0013(3) 0.0136(3) 0.0051(3)
Cl2 0.0490(5) 0.0372(4) 0.0302(4) -0.0033(3) 0.0038(3) -0.0176(4)
Cl3 0.0917(8) 0.0428(5) 0.0248(4) 0.0071(4) -0.0032(4) 0.0200(5)
Cl4 0.0307(4) 0.0802(7) 0.0499(5) -0.0350(5) 0.0183(4) -0.0093(4)
C11 0.023(3) 0.027(2) 0.018(2) 0.0009(17) 0.0061(19) 0.0018(19)
C21 0.024(3) 0.039(3) 0.028(2) -0.010(2) 0.014(2) -0.009(2)
C12 0.024(7) 0.046(8) 0.019(5) 0.002(5) 0.000(5) -0.010(6)
C22 0.033(8) 0.038(7) 0.027(6) 0.003(5) 0.005(5) -0.008(5)

# MOLECULAR GEOMETRY

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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cl1 C11 1.787(6) . ?
Cl1 C22 1.768(18) . ?
Cl2 C11 1.775(4) . ?
Cl2 C12 1.849(10) . ?
Cl3 C11 1.788(4) . ?
Cl3 C12 1.796(11) . ?
Cl4 C12 1.884(18) . ?
Cl4 C21 1.753(6) . ?
C11 C21 1.527(9) . ?
C12 C22 1.42(3) . ?
C21 H211 0.9700 . ?
C21 H212 0.9700 . ?
C22 H221 0.9700 . ?
C22 H222 0.9700 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C21 C11 Cl2 109.0(4) . . ?
C21 C11 Cl3 108.8(4) . . ?
Cl2 C11 Cl3 107.7(2) . . ?
C21 C11 Cl1 106.0(3) . . ?
Cl2 C11 Cl1 113.2(3) . . ?
Cl1 C11 Cl3 112.0(3) . . ?
C11 C21 Cl4 110.4(4) . . ?
C11 C21 H211 109.6 . . ?
Cl4 C21 H211 109.6 . . ?
C11 C21 H212 109.6 . . ?
Cl4 C21 H212 109.6 . . ?
H211 C21 H212 108.1 . . ?
C22 C12 Cl3 108.1(12) . . ?
C22 C12 Cl2 105.2(11) . . ?
Cl3 C12 Cl2 104.2(6) . . ?
C22 C12 Cl4 103.8(10) . . ?
Cl3 C12 Cl4 118.1(8) . . ?
Cl2 C12 Cl4 116.5(8) . . ?
C12 C22 Cl1 108.4(11) . . ?
C12 C22 H221 110.0 . . ?
Cl1 C22 H221 110.0 . . ?
C12 C22 H222 110.0 . . ?
Cl1 C22 H222 110.0 . . ?
H221 C22 H222 108.4 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Cl2 C11 C21 Cl4 59.4(4) . . . . ?
Cl3 C11 C21 Cl4 -57.8(4) . . . . ?
Cl1 C11 C21 Cl4 -178.4(2) . . . . ?
Cl3 C12 C22 Cl1 53.6(10) . . . . ?
Cl2 C12 C22 Cl1 -57.3(9) . . . . ?
Cl4 C12 C22 Cl1 179.9(5) . . . . ?

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         0.616
_refine_diff_density_min         -0.592
_refine_diff_density_rms         0.056

#############################################################################

data_1112TCE_105GPa
_database_code_depnum_ccdc_archive 'CCDC 746846'
#TrackingRef '1112TCE_CIF_LT_HPall16.cif'

# CHEMICAL DATA

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
1,1,2,2-tetrachloroethane
;
_chemical_name_common            1,1,2,2-tetrachloroethane
_chemical_melting_point          ?
_chemical_formula_moiety         'C2 H2 Cl4'
_chemical_formula_sum            'C2 H2 Cl4'
_chemical_formula_weight         167.84

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

# CRYSTAL DATA

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/c'
_symmetry_space_group_name_Hall  '-P 2ybc'

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

_cell_length_a                   5.7549(14)
_cell_length_b                   11.979(7)
_cell_length_c                   8.734(5)
_cell_angle_alpha                90.00
_cell_angle_beta                 110.32(4)
_cell_angle_gamma                90.00
_cell_volume                     564.6(5)
_cell_formula_units_Z            4
_cell_measurement_temperature    295(2)
_cell_measurement_reflns_used    2929
_cell_measurement_theta_min      3.01
_cell_measurement_theta_max      27.48

_exptl_crystal_description       cylinder
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.44
_exptl_crystal_size_mid          0.43
_exptl_crystal_size_min          0.25
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.974
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             328
_exptl_absorpt_coefficient_mu    1.939
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_correction_T_min  0.63
_exptl_absorpt_correction_T_max  0.68
_exptl_absorpt_process_details   
;
Correction for absorption of the diamond-anvil cell and the sample
were made using program REDSHABS (Katrusiak, A. (2003) REDSHABS. Adam
Mickiewicz University Poznań; Katrusiak, A. (2004) Z. Kristallogr.
219, 461-467).
;

# EXPERIMENTAL DATA

_exptl_special_details           
;
Data were collected at room temperature and pressure of 1.05(5) GPa
(1050000 kPa) with the crystal obtained by the in-situ high-pressure
crystallization technique.
Pressure was determined by monitoring the shift of the ruby
R1-fluorescence line.
;

_diffrn_ambient_temperature      295(2)
_diffrn_ambient_environment      'diamond-anvil cell'
_diffrn_ambient_pressure         1050000
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'KM-4 CCD'
_diffrn_measurement_method       'φ- and ω-scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        0
_diffrn_reflns_number            3635
_diffrn_reflns_av_R_equivalents  0.2175
_diffrn_reflns_av_sigmaI/netI    0.2842
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_theta_min         3.01
_diffrn_reflns_theta_max         24.96
_reflns_number_total             515
_reflns_number_gt                488
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'CrysAlisCCD (Oxford Diffraction, 2007)'
_computing_cell_refinement       'CrysAlisRED (Oxford Diffraction, 2007)'
_computing_data_reduction        
'CrysAlisRED (Oxford Diffraction, 2007); REDSHABS (Katrusiak, A. 2003)'
_computing_structure_solution    'SHELXS--97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL--97 (Sheldrick, 1997)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 1990)'
_computing_publication_material  'SHELXL--97 (Sheldrick, 1997)'

# REFINEMENT DATA

_refine_special_details          
;
Refinement of F² against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F², conventional R-factors R are based
on F, with F set to zero for negative F². The threshold expression of
F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F² are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.

The DAC imposes severe restrictions on which reflections can be collected,
resulting in a low data:parameter ratio.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.1035P)²+2.3159P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         515
_refine_ls_number_parameters     55
_refine_ls_number_restraints     12
_refine_ls_R_factor_all          0.1269
_refine_ls_R_factor_gt           0.0861
_refine_ls_wR_factor_ref         0.2024
_refine_ls_wR_factor_gt          0.1978
_refine_ls_goodness_of_fit_ref   1.155
_refine_ls_restrained_S_all      1.142
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

# ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Cl1 Cl 0.4180(4) 0.7738(3) 0.3084(3) 0.0540(9) Uani 1 1 d . . .
Cl2 Cl 0.0118(4) 0.6574(3) 0.0681(3) 0.0521(9) Uani 1 1 d . . .
Cl3 Cl 0.5010(4) 0.5588(2) 0.1913(4) 0.0538(10) Uani 1 1 d . . .
Cl4 Cl 0.1121(4) 0.4516(2) 0.3398(3) 0.0460(9) Uani 1 1 d . . .
C1 C 0.2864(14) 0.6408(8) 0.2415(11) 0.033(2) Uani 1 1 d U . .
C2 C 0.2259(16) 0.5903(8) 0.3837(12) 0.039(2) Uani 1 1 d U . .
H21 H 0.1026 0.6360 0.4063 0.047 Uiso 1 1 calc R . .
H22 H 0.3741 0.5900 0.4805 0.047 Uiso 1 1 calc R . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Cl1 0.0552(14) 0.041(3) 0.060(3) -0.0047(10) 0.0122(13) -0.0115(12)
Cl2 0.0426(12) 0.066(3) 0.037(3) 0.0118(10) -0.0001(11) -0.0057(11)
Cl3 0.0570(15) 0.057(3) 0.065(3) 0.0043(11) 0.0433(15) 0.0102(12)
Cl4 0.0542(14) 0.044(3) 0.045(2) -0.0006(9) 0.0236(12) -0.0085(11)
C1 0.033(4) 0.033(6) 0.034(6) 0.002(3) 0.012(4) 0.006(3)
C2 0.044(4) 0.033(7) 0.041(6) -0.004(3) 0.014(4) -0.003(4)

# MOLECULAR GEOMETRY

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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cl1 C1 1.774(10) . ?
Cl2 C1 1.780(8) . ?
Cl3 C1 1.749(9) . ?
Cl4 C2 1.778(10) . ?
C1 C2 1.527(13) . ?
C2 H21 0.9700 . ?
C2 H22 0.9700 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C2 C1 Cl3 111.2(6) . . ?
C2 C1 Cl1 106.3(6) . . ?
Cl3 C1 Cl1 109.2(4) . . ?
C2 C1 Cl2 110.5(6) . . ?
Cl3 C1 Cl2 110.2(5) . . ?
Cl1 C1 Cl2 109.4(5) . . ?
C1 C2 Cl4 111.5(7) . . ?
C1 C2 H21 109.3 . . ?
Cl4 C2 H21 109.3 . . ?
C1 C2 H22 109.3 . . ?
Cl4 C2 H22 109.3 . . ?
H21 C2 H22 108.0 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Cl3 C1 C2 Cl4 -57.0(8) . . . . ?
Cl1 C1 C2 Cl4 -175.8(4) . . . . ?
Cl2 C1 C2 Cl4 65.6(7) . . . . ?

_diffrn_measured_fraction_theta_max 0.520
_diffrn_reflns_theta_full        24.96
_diffrn_measured_fraction_theta_full 0.520
_refine_diff_density_max         0.471
_refine_diff_density_min         -0.423
_refine_diff_density_rms         0.124

#############################################################################

data_1112TCE_165GPa
_database_code_depnum_ccdc_archive 'CCDC 746847'
#TrackingRef '1112TCE_CIF_LT_HPall16.cif'

# CHEMICAL DATA

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
1,1,2,2-tetrachloroethane
;
_chemical_name_common            1,1,2,2-tetrachloroethane
_chemical_melting_point          ?
_chemical_formula_moiety         'C2 H2 Cl4'
_chemical_formula_sum            'C2 H2 Cl4'
_chemical_formula_weight         167.84

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

# CRYSTAL DATA

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/c'
_symmetry_space_group_name_Hall  '-P 2ybc'

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

_cell_length_a                   5.6957(14)
_cell_length_b                   11.850(7)
_cell_length_c                   8.610(5)
_cell_angle_alpha                90.00
_cell_angle_beta                 110.35(4)
_cell_angle_gamma                90.00
_cell_volume                     544.9(5)
_cell_formula_units_Z            4
_cell_measurement_temperature    295(2)
_cell_measurement_reflns_used    3282
_cell_measurement_theta_min      3.05
_cell_measurement_theta_max      28.18

_exptl_crystal_description       cylinder
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.44
_exptl_crystal_size_mid          0.44
_exptl_crystal_size_min          0.25
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.046
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             328
_exptl_absorpt_coefficient_mu    2.009
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_correction_T_min  0.54
_exptl_absorpt_correction_T_max  0.60
_exptl_absorpt_process_details   
;
Correction for absorption of the diamond-anvil cell and the sample
were made using program REDSHABS (Katrusiak, A. (2003) REDSHABS. Adam
Mickiewicz University Poznań; Katrusiak, A. (2004) Z. Kristallogr.
219, 461-467).
;

# EXPERIMENTAL DATA

_exptl_special_details           
;
Data were collected at room temperature and pressure of 1.65(5) GPa
(1650000 kPa) with the crystal obtained by the in-situ high-pressure
crystallization technique.
Pressure was determined by monitoring the shift of the ruby
R1-fluorescence line.
;

_diffrn_ambient_temperature      295(2)
_diffrn_ambient_environment      'diamond-anvil cell'
_diffrn_ambient_pressure         1650000
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'KM-4 CCD'
_diffrn_measurement_method       'φ- and ω-scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        0
_diffrn_reflns_number            3565
_diffrn_reflns_av_R_equivalents  0.1536
_diffrn_reflns_av_sigmaI/netI    0.0629
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_theta_min         3.05
_diffrn_reflns_theta_max         25.00
_reflns_number_total             500
_reflns_number_gt                478
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'CrysAlisCCD (Oxford Diffraction, 2007)'
_computing_cell_refinement       'CrysAlisRED (Oxford Diffraction, 2007)'
_computing_data_reduction        
'CrysAlisRED (Oxford Diffraction, 2007); REDSHABS (Katrusiak, A. 2003)'
_computing_structure_solution    'SHELXS--97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL--97 (Sheldrick, 1997)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 1990)'
_computing_publication_material  'SHELXL--97 (Sheldrick, 1997)'

# REFINEMENT DATA

_refine_special_details          
;
Refinement of F² against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F², conventional R-factors R are based
on F, with F set to zero for negative F². The threshold expression of
F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F² are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.

The DAC imposes severe restrictions on which reflections can be collected,
resulting in a low data:parameter ratio.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.1014P)²+0.9441P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         500
_refine_ls_number_parameters     55
_refine_ls_number_restraints     12
_refine_ls_R_factor_all          0.0713
_refine_ls_R_factor_gt           0.0691
_refine_ls_wR_factor_ref         0.1729
_refine_ls_wR_factor_gt          0.1707
_refine_ls_goodness_of_fit_ref   1.180
_refine_ls_restrained_S_all      1.165
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

# ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Cl1 Cl 0.4212(3) 0.77469(18) 0.3103(3) 0.0452(7) Uani 1 1 d . . .
Cl2 Cl 0.0107(3) 0.65811(19) 0.0659(2) 0.0444(8) Uani 1 1 d . . .
Cl3 Cl 0.5053(3) 0.55792(18) 0.1910(3) 0.0449(8) Uani 1 1 d . . .
Cl4 Cl 0.1124(3) 0.44924(17) 0.3409(3) 0.0386(7) Uani 1 1 d . . .
C1 C 0.2859(11) 0.6401(6) 0.2425(9) 0.0286(17) Uani 1 1 d U . .
C2 C 0.2227(12) 0.5892(6) 0.3839(10) 0.0333(18) Uani 1 1 d U . .
H21 H 0.0957 0.6349 0.4049 0.040 Uiso 1 1 calc R . .
H22 H 0.3708 0.5898 0.4832 0.040 Uiso 1 1 calc R . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Cl1 0.0461(11) 0.033(2) 0.051(2) -0.0055(7) 0.0104(10) -0.0094(8)
Cl2 0.0360(10) 0.055(2) 0.033(2) 0.0105(7) 0.0007(9) -0.0053(8)
Cl3 0.0478(11) 0.046(2) 0.056(2) 0.0041(8) 0.0373(11) 0.0100(8)
Cl4 0.0436(10) 0.036(2) 0.040(2) -0.0011(7) 0.0202(10) -0.0080(7)
C1 0.025(3) 0.025(6) 0.036(6) 0.001(2) 0.010(3) 0.000(3)
C2 0.038(3) 0.035(7) 0.030(7) -0.002(3) 0.016(3) 0.002(3)

# MOLECULAR GEOMETRY

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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cl1 C1 1.779(8) . ?
Cl2 C1 1.777(7) . ?
Cl3 C1 1.759(7) . ?
Cl4 C2 1.766(8) . ?
C1 C2 1.510(10) . ?
C2 H21 0.9700 . ?
C2 H22 0.9700 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C2 C1 Cl3 111.8(5) . . ?
C2 C1 Cl2 110.5(4) . . ?
Cl3 C1 Cl2 110.1(4) . . ?
C2 C1 Cl1 106.9(5) . . ?
Cl3 C1 Cl1 108.3(3) . . ?
Cl2 C1 Cl1 109.0(4) . . ?
C1 C2 Cl4 111.9(5) . . ?
C1 C2 H21 109.2 . . ?
Cl4 C2 H21 109.2 . . ?
C1 C2 H22 109.2 . . ?
Cl4 C2 H22 109.2 . . ?
H21 C2 H22 107.9 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Cl3 C1 C2 Cl4 -56.2(6) . . . . ?
Cl2 C1 C2 Cl4 66.8(5) . . . . ?
Cl1 C1 C2 Cl4 -174.6(3) . . . . ?

_diffrn_measured_fraction_theta_max 0.521
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.521
_refine_diff_density_max         0.434
_refine_diff_density_min         -0.428
_refine_diff_density_rms         0.116

#############################################################################

data_1112TCE_255GPa
_database_code_depnum_ccdc_archive 'CCDC 746848'
#TrackingRef '1112TCE_CIF_LT_HPall16.cif'

# CHEMICAL DATA

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
1,1,2,2-tetrachloroethane
;
_chemical_name_common            1,1,2,2-tetrachloroethane
_chemical_melting_point          ?
_chemical_formula_moiety         'C2 H2 Cl4'
_chemical_formula_sum            'C2 H2 Cl4'
_chemical_formula_weight         167.84

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

# CRYSTAL DATA

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/c'
_symmetry_space_group_name_Hall  '-P 2ybc'

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

_cell_length_a                   5.5937(14)
_cell_length_b                   11.586(6)
_cell_length_c                   8.336(5)
_cell_angle_alpha                90.00
_cell_angle_beta                 110.60(4)
_cell_angle_gamma                90.00
_cell_volume                     505.7(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    295(2)
_cell_measurement_reflns_used    2858
_cell_measurement_theta_min      3.14
_cell_measurement_theta_max      28.90

_exptl_crystal_description       cylinder
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.43
_exptl_crystal_size_mid          0.43
_exptl_crystal_size_min          0.25
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.204
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             328
_exptl_absorpt_coefficient_mu    2.164
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_correction_T_min  0.54
_exptl_absorpt_correction_T_max  0.59
_exptl_absorpt_process_details   
;
Correction for absorption of the diamond-anvil cell and the sample
were made using program REDSHABS (Katrusiak, A. (2003) REDSHABS. Adam
Mickiewicz University Poznań; Katrusiak, A. (2004) Z. Kristallogr.
219, 461-467).
;

# EXPERIMENTAL DATA

_exptl_special_details           
;
Data were collected at room temperature and pressure of 2.55(5) GPa
(2550000 kPa) with the crystal obtained by the in-situ high-pressure
crystallization technique.
Pressure was determined by monitoring the shift of the ruby
R1-fluorescence line.
;

_diffrn_ambient_temperature      295(2)
_diffrn_ambient_environment      'diamond-anvil cell'
_diffrn_ambient_pressure         2550000
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'KM-4 CCD'
_diffrn_measurement_method       'φ- and ω-scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        0
_diffrn_reflns_number            3193
_diffrn_reflns_av_R_equivalents  0.2712
_diffrn_reflns_av_sigmaI/netI    0.1002
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_theta_min         3.15
_diffrn_reflns_theta_max         24.90
_reflns_number_total             443
_reflns_number_gt                404
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'CrysAlisCCD (Oxford Diffraction, 2007)'
_computing_cell_refinement       'CrysAlisRED (Oxford Diffraction, 2007)'
_computing_data_reduction        
'CrysAlisRED (Oxford Diffraction, 2007); REDSHABS (Katrusiak, A. 2003)'
_computing_structure_solution    'SHELXS--97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL--97 (Sheldrick, 1997)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 1990)'
_computing_publication_material  'SHELXL--97 (Sheldrick, 1997)'

# REFINEMENT DATA

_refine_special_details          
;
Refinement of F² against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F², conventional R-factors R are based
on F, with F set to zero for negative F². The threshold expression of
F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F² are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.

The DAC imposes severe restrictions on which reflections can be collected,
resulting in a low data:parameter ratio.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.1535P)²+0.9252P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         443
_refine_ls_number_parameters     55
_refine_ls_number_restraints     12
_refine_ls_R_factor_all          0.0973
_refine_ls_R_factor_gt           0.0901
_refine_ls_wR_factor_ref         0.2365
_refine_ls_wR_factor_gt          0.2272
_refine_ls_goodness_of_fit_ref   1.154
_refine_ls_restrained_S_all      1.140
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

# ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Cl1 Cl 0.4258(4) 0.7769(3) 0.3145(4) 0.0417(11) Uani 1 1 d . . .
Cl2 Cl 0.0091(4) 0.6591(3) 0.0610(3) 0.0402(11) Uani 1 1 d . . .
Cl3 Cl 0.5118(4) 0.5567(2) 0.1910(4) 0.0402(10) Uani 1 1 d . . .
Cl4 Cl 0.1140(4) 0.4442(2) 0.3426(4) 0.0379(10) Uani 1 1 d . . .
C1 C 0.2885(14) 0.6432(9) 0.2431(14) 0.030(2) Uani 1 1 d U . .
C2 C 0.2214(17) 0.5857(10) 0.3882(16) 0.039(3) Uani 1 1 d U . .
H21 H 0.0902 0.6310 0.4100 0.047 Uiso 1 1 calc R . .
H22 H 0.3715 0.5862 0.4918 0.047 Uiso 1 1 calc R . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Cl1 0.0360(14) 0.036(3) 0.049(3) -0.0052(9) 0.0109(13) -0.0064(10)
Cl2 0.0290(13) 0.048(3) 0.038(3) 0.0075(9) 0.0047(13) -0.0045(9)
Cl3 0.0434(14) 0.035(3) 0.055(3) 0.0037(10) 0.0329(15) 0.0069(10)
Cl4 0.0381(14) 0.037(3) 0.043(3) -0.0008(9) 0.0198(14) -0.0084(10)
C1 0.017(4) 0.032(9) 0.041(9) 0.005(3) 0.010(4) 0.002(4)
C2 0.030(4) 0.035(10) 0.054(10) -0.005(4) 0.017(5) -0.011(4)

# MOLECULAR GEOMETRY

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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cl1 C1 1.739(11) . ?
Cl2 C1 1.764(9) . ?
Cl3 C1 1.770(10) . ?
Cl4 C2 1.741(11) . ?
C1 C2 1.537(15) . ?
C2 H21 0.9700 . ?
C2 H22 0.9700 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C2 C1 Cl1 108.5(8) . . ?
C2 C1 Cl2 109.5(6) . . ?
Cl1 C1 Cl2 110.6(5) . . ?
C2 C1 Cl3 109.7(7) . . ?
Cl1 C1 Cl3 108.9(4) . . ?
Cl2 C1 Cl3 109.6(6) . . ?
C1 C2 Cl4 113.4(8) . . ?
C1 C2 H21 108.9 . . ?
Cl4 C2 H21 108.9 . . ?
C1 C2 H22 108.9 . . ?
Cl4 C2 H22 108.9 . . ?
H21 C2 H22 107.7 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Cl1 C1 C2 Cl4 -173.4(5) . . . . ?
Cl2 C1 C2 Cl4 65.7(8) . . . . ?
Cl3 C1 C2 Cl4 -54.6(8) . . . . ?

_diffrn_measured_fraction_theta_max 0.503
_diffrn_reflns_theta_full        24.90
_diffrn_measured_fraction_theta_full 0.503
_refine_diff_density_max         0.746
_refine_diff_density_min         -0.541
_refine_diff_density_rms         0.178

#############################################################################


