# 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
#TrackingRef '- 111TCE.cif'
_audit_update_record
;
2010-07-16 # Formatted by publCIF
;
_audit_creation_method SHELXL-97
# PROCESSING SUMMARY ( IUCr Office Use Only)
_journal_date_recd_electronic ?
_journal_date_from_coeditor ?
_journal_date_accepted ?
_journal_coeditor_code ?
# SUBMISSION DETAILS
_publ_contact_author_name 'Andrzej Katrusiak'
_publ_contact_author_address
; Faculty of Chemistry
Adam Mickiewicz University
Grunwaldzka 6
60-780 Pozna\'n
Poland
;
_publ_contact_author_email katran@amu.edu.pl
_publ_contact_letter
; Please consider this CIF submission for publication in
Chemical Communications
;
_publ_requested_category FO
_publ_requested_coeditor_name ?
# TITLE AND AUTHOR LIST
_publ_section_title
;
Crystalline gas of 1,1,1-trichloroethane
;
loop_
_publ_author_name
_publ_author_address
M.Bujak
; Faculty of Chemistry
University of Opole
Oleska 48
45-052 Opole
Poland
;
M.Podsiadlo
; Faculty of Chemistry
Adam Mickiewicz University
Grunwaldzka 6
60-780 Pozna\'n
Poland
;
A.Katrusiak
; Faculty of Chemistry
Adam Mickiewicz University
Grunwaldzka 6
60-780 Pozna\'n
Poland
;
#############################################################################
data_111TCE_220K
_database_code_depnum_ccdc_archive 'CCDC 784823'
#TrackingRef '- 111TCE.cif'
# CHEMICAL DATA
_audit_creation_method SHELXL-97
_chemical_name_systematic
;
1,1,1-trichloroethane
;
_chemical_name_common 1,1,1-trichloroethane
_chemical_melting_point 242.8
_chemical_formula_moiety 'C2 H3 Cl3'
_chemical_formula_sum 'C2 H3 Cl3'
_chemical_formula_weight 133.39
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 orthorhombic
_symmetry_space_group_name_H-M 'P n m a'
_symmetry_space_group_name_Hall '-P 2ac 2n'
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z'
'x+1/2, -y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z'
'-x-1/2, y-1/2, z-1/2'
_cell_length_a 11.5520(10)
_cell_length_b 8.0069(7)
_cell_length_c 5.8733(4)
_cell_angle_alpha 90.00
_cell_angle_beta 90.00
_cell_angle_gamma 90.00
_cell_volume 543.26(8)
_cell_formula_units_Z 4
_cell_measurement_temperature 220.0(1)
_cell_measurement_pressure 100
_cell_measurement_reflns_used 804
_cell_measurement_theta_min 3.09
_cell_measurement_theta_max 28.97
_exptl_crystal_description irregular
_exptl_crystal_colour colourless
_exptl_crystal_size_max 0.30
_exptl_crystal_size_mid 0.30
_exptl_crystal_size_min 0.10
_exptl_crystal_density_meas ?
_exptl_crystal_density_diffrn 1.631
_exptl_crystal_density_method 'not measured'
_exptl_crystal_F_000 264
_exptl_absorpt_coefficient_mu 1.516
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_correction_T_min 0.6591
_exptl_absorpt_correction_T_max 0.8632
_exptl_absorpt_process_details
;
Correction for absorption was made using CrysAlisPro,
Oxford Diffraction Ltd. (2009)
;
_exptl_special_details
;
Data were collected at ambient pressure (100 kPa) and 220.0(1) K with the
crystal obtained by the in-situ low-temperature crystallization
technique.
;
# EXPERIMENTAL DATA
_diffrn_ambient_temperature 220.0(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 'Oxford Diffraction Xcalibur E'
_diffrn_measurement_method \w-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 1302
_diffrn_reflns_av_R_equivalents 0.0184
_diffrn_reflns_av_sigmaI/netI 0.0234
_diffrn_reflns_limit_h_min -4
_diffrn_reflns_limit_h_max 13
_diffrn_reflns_limit_k_min -9
_diffrn_reflns_limit_k_max 4
_diffrn_reflns_limit_l_min -4
_diffrn_reflns_limit_l_max 7
_diffrn_reflns_theta_min 3.53
_diffrn_reflns_theta_max 25.03
_reflns_number_total 515
_reflns_number_gt 393
_reflns_threshold_expression I>2\s(I)
_computing_data_collection 'CrysAlisPro (Oxford Diffraction Ltd, 2009)'
_computing_cell_refinement 'CrysAlisPro (Oxford Diffraction Ltd, 2009)'
_computing_data_reduction 'CrysAlisPro (Oxford Diffraction Ltd, 2009)'
_computing_structure_solution 'SHELXS--97 (Sheldrick, 2008)'
_computing_structure_refinement 'SHELXL--97 (Sheldrick, 2008)'
_computing_molecular_graphics 'Mercury (Macrae at al., 2008)'
_computing_publication_material 'SHELXL--97 (Sheldrick, 2008)'
# REFINEMENT DATA
_refine_special_details
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ 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/[\s^2^(Fo^2^)+(0.0544P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_atom_sites_solution_hydrogens difmap
_refine_ls_hydrogen_treatment mixed
_refine_ls_extinction_method none
_refine_ls_extinction_coef ?
_refine_ls_number_reflns 515
_refine_ls_number_parameters 33
_refine_ls_number_restraints 2
_refine_ls_R_factor_all 0.0432
_refine_ls_R_factor_gt 0.0329
_refine_ls_wR_factor_ref 0.0866
_refine_ls_wR_factor_gt 0.0837
_refine_ls_goodness_of_fit_ref 0.999
_refine_ls_restrained_S_all 1.003
_refine_ls_shift/su_max 0.000
_refine_ls_shift/su_mean 0.000
_publ_section_exptl_refinement
;
All hydrogen atoms, in the low-temperature structure at 220 K/0.1 MPa, were
located in the subsequent difference Fourier maps, refined and geometrically
restrained to the same distance (DFIX command of SHELXL97). The
positions of H-atoms, in the high-pressure structures, were taken from the
low-temperature model and refined using geometrical restrains similar to the
low-temperature structure refinement. The H-atoms displacement parameters, in
all structures, were taken with coefficients 1.5 times larger than the
respective parameters of the C atoms.
;
# 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 0.65382(7) 0.07124(10) 0.19135(13) 0.0628(3) Uani 1 1 d . . .
Cl2 Cl 0.61834(11) 0.2500 0.60763(15) 0.0656(4) Uani 1 2 d S . .
C1 C 0.5873(3) 0.2500 0.3119(5) 0.0395(8) Uani 1 2 d S . .
C2 C 0.4599(4) 0.2500 0.2702(8) 0.0587(11) Uani 1 2 d SD . .
H1 H 0.444(4) 0.2500 0.109(3) 0.088 Uiso 1 2 d SD . .
H2 H 0.428(3) 0.152(3) 0.338(5) 0.088 Uiso 1 1 d D . .
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 0.0643(5) 0.0580(5) 0.0663(6) -0.0176(3) 0.0014(3) 0.0136(4)
Cl2 0.0916(9) 0.0687(7) 0.0365(6) 0.000 -0.0037(5) 0.000
C1 0.043(2) 0.041(2) 0.0353(17) 0.000 0.0031(14) 0.000
C2 0.039(2) 0.055(3) 0.081(3) 0.000 -0.009(2) 0.000
# 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 1.772(2) . ?
Cl2 C1 1.773(3) . ?
C1 C2 1.492(5) . ?
C2 H1 0.96(2) . ?
C2 H2 0.96(1) . ?
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 111.22(16) . . ?
Cl1 C1 Cl1 107.75(18) 7_565 . ?
C2 C1 Cl2 111.1(3) . . ?
Cl1 C1 Cl2 107.69(14) . . ?
C1 C2 H1 110(3) . . ?
C1 C2 H2 108(2) . . ?
H1 C2 H2 110(2) . . ?
_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full 25.03
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max 0.313
_refine_diff_density_min -0.250
_refine_diff_density_rms 0.060
#############################################################################
data_111TCE_0.75GPa
_database_code_depnum_ccdc_archive 'CCDC 784824'
#TrackingRef '- 111TCE.cif'
# CHEMICAL DATA
_audit_creation_method SHELXL-97
_chemical_name_systematic
;
1,1,1-trichloroethane
;
_chemical_name_common 1,1,1-trichloroethane
_chemical_melting_point 242.8
_chemical_formula_moiety 'C2 H3 Cl3'
_chemical_formula_sum 'C2 H3 Cl3'
_chemical_formula_weight 133.39
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 orthorhombic
_symmetry_space_group_name_H-M 'P n m a'
_symmetry_space_group_name_Hall '-P 2ac 2n'
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z'
'x+1/2, -y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z'
'-x-1/2, y-1/2, z-1/2'
_cell_length_a 11.266(2)
_cell_length_b 7.748(8)
_cell_length_c 5.7183(12)
_cell_angle_alpha 90.00
_cell_angle_beta 90.00
_cell_angle_gamma 90.00
_cell_volume 499.1(5)
_cell_formula_units_Z 4
_cell_measurement_temperature 295(2)
_cell_measurement_pressure 750000
_cell_measurement_reflns_used 1471
_cell_measurement_theta_min 3.61
_cell_measurement_theta_max 27.01
_exptl_crystal_description prism
_exptl_crystal_colour colourless
_exptl_crystal_size_max 0.36
_exptl_crystal_size_mid 0.22
_exptl_crystal_size_min 0.20
_exptl_crystal_density_meas ?
_exptl_crystal_density_diffrn 1.775
_exptl_crystal_density_method 'not measured'
_exptl_crystal_F_000 264
_exptl_absorpt_coefficient_mu 1.650
_exptl_absorpt_correction_type numerical
_exptl_absorpt_correction_T_min 0.239
_exptl_absorpt_correction_T_max 0.665
_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 Pozna\'n; Katrusiak, A. (2004) Z. Kristallogr.
219, 461-467).
;
# EXPERIMENTAL DATA
_exptl_special_details
;
Data were collected at room temperature and pressure of 0.75(5) GPa (750000 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 750000
_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 '\f- and \w-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 2106
_diffrn_reflns_av_R_equivalents 0.1432
_diffrn_reflns_av_sigmaI/netI 0.0507
_diffrn_reflns_limit_h_min -12
_diffrn_reflns_limit_h_max 12
_diffrn_reflns_limit_k_min -4
_diffrn_reflns_limit_k_max 4
_diffrn_reflns_limit_l_min -6
_diffrn_reflns_limit_l_max 6
_diffrn_reflns_theta_min 3.62
_diffrn_reflns_theta_max 25.05
_reflns_number_total 213
_reflns_number_gt 203
_reflns_threshold_expression I>2\s(I)
_computing_data_collection 'CrysAlisCCD (Oxford Diffraction Ltd, 2009)'
_computing_cell_refinement 'CrysAlisRED (Oxford Diffraction Ltd, 2009)'
_computing_data_reduction
'CrysAlisRED (Oxford Diffraction Ltd, 2009); REDSHABS (Katrusiak, A., 2003)'
_computing_structure_solution 'SHELXS--97 (Sheldrick, 2008)'
_computing_structure_refinement 'SHELXL--97 (Sheldrick, 2008)'
_computing_molecular_graphics 'Mercury (Macrae at al., 2008)'
_computing_publication_material 'SHELXL--97 (Sheldrick, 2008)'
# REFINEMENT DATA
_refine_special_details
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ 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/[\s^2^(Fo^2^)+(0.0203P)^2^+1.4299P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_atom_sites_solution_hydrogens geom
_refine_ls_hydrogen_treatment mixed
_refine_ls_extinction_method SHELXL
_refine_ls_extinction_coef 0.21(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_number_reflns 213
_refine_ls_number_parameters 34
_refine_ls_number_restraints 14
_refine_ls_R_factor_all 0.0628
_refine_ls_R_factor_gt 0.0586
_refine_ls_wR_factor_ref 0.1141
_refine_ls_wR_factor_gt 0.1130
_refine_ls_goodness_of_fit_ref 1.256
_refine_ls_restrained_S_all 1.222
_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 0.65244(16) 0.0641(5) 0.1905(3) 0.0551(18) Uani 1 1 d . . .
Cl2 Cl 0.6172(3) 0.2500 0.6184(4) 0.056(3) Uani 1 2 d S . .
C1 C 0.5861(7) 0.2500 0.3134(14) 0.037(4) Uani 1 2 d SU . .
C2 C 0.4523(9) 0.2500 0.2743(19) 0.045(4) Uani 1 2 d SDU . .
H1 H 0.439(8) 0.2500 0.109(4) 0.068 Uiso 1 2 d SD . .
H2 H 0.421(7) 0.146(6) 0.339(12) 0.068 Uiso 1 1 d D . .
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 0.0561(16) 0.052(6) 0.0575(13) -0.0151(15) 0.0024(7) 0.0111(15)
Cl2 0.081(2) 0.053(8) 0.0333(14) 0.000 -0.0049(10) 0.000
C1 0.038(5) 0.040(11) 0.032(4) 0.000 0.002(3) 0.000
C2 0.037(5) 0.040(11) 0.059(5) 0.000 -0.008(4) 0.000
# 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 1.768(6) . ?
Cl2 C1 1.779(8) . ?
C1 C2 1.524(13) . ?
C2 H1 0.96(2) . ?
C2 H2 0.96(2) . ?
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C2 C1 Cl1 111.1(4) . . ?
Cl1 C1 Cl1 109.1(5) 7_565 . ?
C2 C1 Cl2 109.8(7) . . ?
Cl1 C1 Cl2 107.8(3) . . ?
C1 C2 H1 108(6) . . ?
C1 C2 H2 108(5) . . ?
H1 C2 H2 109(5) . . ?
_diffrn_measured_fraction_theta_max 0.443
_diffrn_reflns_theta_full 25.05
_diffrn_measured_fraction_theta_full 0.443
_refine_diff_density_max 0.242
_refine_diff_density_min -0.306
_refine_diff_density_rms 0.062
#############################################################################
data_111TCE_1.15GPa
_database_code_depnum_ccdc_archive 'CCDC 784825'
#TrackingRef '- 111TCE.cif'
# CHEMICAL DATA
_audit_creation_method SHELXL-97
_chemical_name_systematic
;
1,1,1-trichloroethane
;
_chemical_name_common 1,1,1-trichloroethane
_chemical_melting_point 242.8
_chemical_formula_moiety 'C2 H3 Cl3'
_chemical_formula_sum 'C2 H3 Cl3'
_chemical_formula_weight 133.39
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 orthorhombic
_symmetry_space_group_name_H-M 'P n m a'
_symmetry_space_group_name_Hall '-P 2ac 2n'
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z'
'x+1/2, -y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z'
'-x-1/2, y-1/2, z-1/2'
_cell_length_a 11.0912(19)
_cell_length_b 7.588(7)
_cell_length_c 5.6253(10)
_cell_angle_alpha 90.00
_cell_angle_beta 90.00
_cell_angle_gamma 90.00
_cell_volume 473.4(5)
_cell_formula_units_Z 4
_cell_measurement_temperature 295(2)
_cell_measurement_pressure 1150000
_cell_measurement_reflns_used 1649
_cell_measurement_theta_min 3.61
_cell_measurement_theta_max 27.47
_exptl_crystal_description prism
_exptl_crystal_colour colourless
_exptl_crystal_size_max 0.35
_exptl_crystal_size_mid 0.23
_exptl_crystal_size_min 0.22
_exptl_crystal_density_meas ?
_exptl_crystal_density_diffrn 1.872
_exptl_crystal_density_method 'not measured'
_exptl_crystal_F_000 264
_exptl_absorpt_coefficient_mu 1.740
_exptl_absorpt_correction_type numerical
_exptl_absorpt_correction_T_min 0.234
_exptl_absorpt_correction_T_max 0.661
_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 Pozna\'n; Katrusiak, A. (2004) Z. Kristallogr.
219, 461-467).
;
# EXPERIMENTAL DATA
_exptl_special_details
;
Data were collected at room temperature and pressure of 1.15(5) GPa (1150000
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 1150000
_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 '\f- and \w-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 2077
_diffrn_reflns_av_R_equivalents 0.1022
_diffrn_reflns_av_sigmaI/netI 0.0413
_diffrn_reflns_limit_h_min -12
_diffrn_reflns_limit_h_max 12
_diffrn_reflns_limit_k_min -4
_diffrn_reflns_limit_k_max 4
_diffrn_reflns_limit_l_min -6
_diffrn_reflns_limit_l_max 6
_diffrn_reflns_theta_min 4.06
_diffrn_reflns_theta_max 25.09
_reflns_number_total 208
_reflns_number_gt 198
_reflns_threshold_expression I>2\s(I)
_computing_data_collection 'CrysAlisCCD (Oxford Diffraction Ltd, 2009)'
_computing_cell_refinement 'CrysAlisRED (Oxford Diffraction Ltd, 2009)'
_computing_data_reduction
'CrysAlisRED (Oxford Diffraction Ltd, 2009); REDSHABS (Katrusiak, A., 2003)'
_computing_structure_solution 'SHELXS--97 (Sheldrick, 2008)'
_computing_structure_refinement 'SHELXL--97 (Sheldrick, 2008)'
_computing_molecular_graphics 'Mercury (Macrae at al., 2008)'
_computing_publication_material 'SHELXL--97 (Sheldrick, 2008)'
# REFINEMENT DATA
_refine_special_details
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ 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/[\s^2^(Fo^2^)+(0.0712P)^2^+1.0664P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_atom_sites_solution_hydrogens geom
_refine_ls_hydrogen_treatment mixed
_refine_ls_extinction_method SHELXL
_refine_ls_extinction_coef 0.060(18)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_number_reflns 208
_refine_ls_number_parameters 34
_refine_ls_number_restraints 17
_refine_ls_R_factor_all 0.0516
_refine_ls_R_factor_gt 0.0475
_refine_ls_wR_factor_ref 0.1386
_refine_ls_wR_factor_gt 0.1314
_refine_ls_goodness_of_fit_ref 1.223
_refine_ls_restrained_S_all 1.181
_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 0.65165(14) 0.0596(5) 0.1910(3) 0.0453(19) Uani 1 1 d . . .
Cl2 Cl 0.6162(2) 0.2500 0.6269(4) 0.045(2) Uani 1 2 d S . .
C1 C 0.5834(7) 0.2500 0.3181(14) 0.035(4) Uani 1 2 d SU . .
C2 C 0.4480(8) 0.2500 0.2753(16) 0.037(4) Uani 1 2 d SDU . .
H1 H 0.436(7) 0.2500 0.107(3) 0.055 Uiso 1 2 d SD . .
H2 H 0.415(4) 0.1464(14) 0.347(6) 0.055 Uiso 1 1 d D . .
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 0.0451(16) 0.047(6) 0.0434(12) -0.0096(13) 0.0021(6) 0.0090(11)
Cl2 0.064(2) 0.046(7) 0.0263(12) 0.000 -0.0040(9) 0.000
C1 0.030(4) 0.046(11) 0.030(4) 0.000 0.003(3) 0.000
C2 0.036(5) 0.028(11) 0.047(4) 0.000 -0.006(4) 0.000
# 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 1.781(6) . ?
Cl2 C1 1.775(8) . ?
C1 C2 1.521(12) . ?
C2 H1 0.96(2) . ?
C2 H2 0.96(1) . ?
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 Cl2 110.9(6) . . ?
C2 C1 Cl1 110.9(4) . . ?
Cl2 C1 Cl1 107.8(3) . . ?
Cl1 C1 Cl1 108.4(5) 7_565 . ?
C1 C2 H1 107(5) . . ?
C1 C2 H2 108(3) . . ?
H1 C2 H2 111(2) . . ?
_diffrn_measured_fraction_theta_max 0.459
_diffrn_reflns_theta_full 25.09
_diffrn_measured_fraction_theta_full 0.459
_refine_diff_density_max 0.378
_refine_diff_density_min -0.317
_refine_diff_density_rms 0.092
#############################################################################
data_111TCE_2.15GPa
_database_code_depnum_ccdc_archive 'CCDC 784826'
#TrackingRef '- 111TCE.cif'
# CHEMICAL DATA
_audit_creation_method SHELXL-97
_chemical_name_systematic
;
1,1,1-trichloroethane
;
_chemical_name_common 1,1,1-trichloroethane
_chemical_melting_point 242.8
_chemical_formula_moiety 'C2 H3 Cl3'
_chemical_formula_sum 'C2 H3 Cl3'
_chemical_formula_weight 133.39
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 orthorhombic
_symmetry_space_group_name_H-M 'P n m a'
_symmetry_space_group_name_Hall '-P 2ac 2n'
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z'
'x+1/2, -y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z'
'-x-1/2, y-1/2, z-1/2'
_cell_length_a 10.914(2)
_cell_length_b 7.414(6)
_cell_length_c 5.5350(10)
_cell_angle_alpha 90.00
_cell_angle_beta 90.00
_cell_angle_gamma 90.00
_cell_volume 447.9(4)
_cell_formula_units_Z 4
_cell_measurement_temperature 295(2)
_cell_measurement_pressure 2150000
_cell_measurement_reflns_used 1734
_cell_measurement_theta_min 3.68
_cell_measurement_theta_max 28.02
_exptl_crystal_description prism
_exptl_crystal_colour colourless
_exptl_crystal_size_max 0.35
_exptl_crystal_size_mid 0.24
_exptl_crystal_size_min 0.22
_exptl_crystal_density_meas ?
_exptl_crystal_density_diffrn 1.978
_exptl_crystal_density_method 'not measured'
_exptl_crystal_F_000 264
_exptl_absorpt_coefficient_mu 1.839
_exptl_absorpt_correction_type numerical
_exptl_absorpt_correction_T_min 0.237
_exptl_absorpt_correction_T_max 0.645
_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 Pozna\'n; Katrusiak, A. (2004) Z. Kristallogr.
219, 461-467).
;
# EXPERIMENTAL DATA
_exptl_special_details
;
Data were collected at room temperature and pressure of 2.15(5) GPa (2150000
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 2150000
_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 '\f- and \w-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 1996
_diffrn_reflns_av_R_equivalents 0.0993
_diffrn_reflns_av_sigmaI/netI 0.0363
_diffrn_reflns_limit_h_min -12
_diffrn_reflns_limit_h_max 12
_diffrn_reflns_limit_k_min -4
_diffrn_reflns_limit_k_max 4
_diffrn_reflns_limit_l_min -6
_diffrn_reflns_limit_l_max 6
_diffrn_reflns_theta_min 4.13
_diffrn_reflns_theta_max 25.09
_reflns_number_total 199
_reflns_number_gt 193
_reflns_threshold_expression I>2\s(I)
_computing_data_collection 'CrysAlisCCD (Oxford Diffraction Ltd, 2009)'
_computing_cell_refinement 'CrysAlisRED (Oxford Diffraction Ltd, 2009)'
_computing_data_reduction
'CrysAlisRED (Oxford Diffraction Ltd, 2009); REDSHABS (Katrusiak, A., 2003)'
_computing_structure_solution 'SHELXS--97 (Sheldrick, 2008)'
_computing_structure_refinement 'SHELXL--97 (Sheldrick, 2008)'
_computing_molecular_graphics 'Mercury (Macrae at al., 2008)'
_computing_publication_material 'SHELXL--97 (Sheldrick, 2008)'
# REFINEMENT DATA
_refine_special_details
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ 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/[\s^2^(Fo^2^)+(0.0650P)^2^+1.6750P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_atom_sites_solution_hydrogens geom
_refine_ls_hydrogen_treatment mixed
_refine_ls_extinction_method SHELXL
_refine_ls_extinction_coef 0.002(7)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_number_reflns 199
_refine_ls_number_parameters 34
_refine_ls_number_restraints 17
_refine_ls_R_factor_all 0.0595
_refine_ls_R_factor_gt 0.0576
_refine_ls_wR_factor_ref 0.1248
_refine_ls_wR_factor_gt 0.1222
_refine_ls_goodness_of_fit_ref 1.136
_refine_ls_restrained_S_all 1.087
_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 0.65125(14) 0.0557(5) 0.1910(2) 0.0331(16) Uani 1 1 d . . .
Cl2 Cl 0.6150(2) 0.2500 0.6347(3) 0.0354(19) Uani 1 2 d S . .
C1 C 0.5833(7) 0.2500 0.3196(13) 0.024(3) Uani 1 2 d SU . .
C2 C 0.4460(8) 0.2500 0.2782(16) 0.030(4) Uani 1 2 d SDU . .
H1 H 0.437(7) 0.2500 0.106(3) 0.044 Uiso 1 2 d SD . .
H2 H 0.410(4) 0.1441(14) 0.346(6) 0.044 Uiso 1 1 d D . .
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 0.0348(14) 0.032(5) 0.0325(10) -0.0076(12) 0.0015(6) 0.0073(9)
Cl2 0.0489(18) 0.039(6) 0.0188(11) 0.000 -0.0037(9) 0.000
C1 0.018(4) 0.030(11) 0.023(3) 0.000 0.002(3) 0.000
C2 0.025(5) 0.028(11) 0.036(4) 0.000 -0.006(3) 0.000
# 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 1.769(5) . ?
Cl2 C1 1.778(7) . ?
C1 C2 1.517(11) . ?
C2 H1 0.96(2) . ?
C2 H2 0.96(1) . ?
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 110.7(4) . . ?
Cl1 C1 Cl1 109.0(4) 7_565 . ?
C2 C1 Cl2 109.9(6) . . ?
Cl1 C1 Cl2 108.2(3) . . ?
C1 C2 H1 105(5) . . ?
C1 C2 H2 111(3) . . ?
H1 C2 H2 110(2) . . ?
_diffrn_measured_fraction_theta_max 0.462
_diffrn_reflns_theta_full 25.09
_diffrn_measured_fraction_theta_full 0.462
_refine_diff_density_max 0.375
_refine_diff_density_min -0.381
_refine_diff_density_rms 0.093
#############################################################################