# Electronic Supplementary Material (ESI) for Chemical Communications
# This journal is © The Royal Society of Chemistry 2011
data_global
_journal_name_full Chem.Commun.
_journal_coden_cambridge 0182
_journal_year ?
_journal_volume ?
_journal_page_first ?
loop_
_publ_author_name
_publ_author_address
M.Bujak
; Faculty of Chemistry
University of Opole
Oleska 48
45-052 Opole
Poland
;
D.Blaser
;
Fachbereich Chemie der
Universit\"at Duisburg-Essen
Campus Essen Universit\"atsstr. 7
D-45117 Essen, Germany
;
A.Katrusiak
; Faculty of Chemistry
Adam Mickiewicz University
Grunwaldzka 6
60-780 Pozna\'n
Poland
;
R.Boese
;
Fachbereich Chemie der
Universit\"at Duisburg-Essen
Campus Essen Universit\"atsstr. 7
D-45117 Essen, Germany
;
# SUBMISSION DETAILS
_publ_contact_author
;
Prof. Dr. Boese, Roland
Fachbereich Chemie der
Universit\"at Duisburg-Essen
Campus Essen, Universit\"atsstr. 7
D-45117 Essen, Germany
;
_publ_contact_author_email roland.boese@.uni-due.de
_publ_contact_author_fax '++49 (0)201 183 2535'
_publ_contact_author_phone '++49 (0)201 183 2416'
_publ_contact_letter
; Please consider this CIF submission for publication in
in The Journal of the American Chemical Society
;
_publ_requested_category FO
_publ_requested_coeditor_name ?
# TITLE AND AUTHOR LIST
_publ_section_title
;
Conformational Polymorphs of 1,1,2,2-Tetrachloroethane: Pressure vs.
Temperature
;
_publ_contact_author_name 'Prof. Dr. Boese, Roland'
data_tcexdb0
_database_code_depnum_ccdc_archive 'CCDC 811781'
#TrackingRef '- 1122TCELThp.cif'
_audit_update_record
;
2010-10-30 # Formatted by publCIF
;
#############################################################################
_ccdc_compound_id 1
# 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 orthorhombic
_symmetry_space_group_name_H-M 'P 21 21 21'
_symmetry_space_group_name_Hall 'P 2ac 2ab'
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
_cell_length_a 8.8687(19)
_cell_length_b 10.501(2)
_cell_length_c 12.835(3)
_cell_angle_alpha 90.00
_cell_angle_beta 90.00
_cell_angle_gamma 90.00
_cell_volume 1195.3(4)
_cell_formula_units_Z 8
_cell_measurement_temperature 215(2)
_cell_measurement_pressure 100
_cell_measurement_reflns_used 3727
_cell_measurement_theta_min 2.49
_cell_measurement_theta_max 28.29
_exptl_crystal_description cylindric
_exptl_crystal_colour colorless
_exptl_crystal_size_max 0.3
_exptl_crystal_size_mid 0.3
_exptl_crystal_size_min 0.3
_exptl_crystal_density_meas ?
_exptl_crystal_density_diffrn 1.865
_exptl_crystal_density_method 'not measured'
_exptl_crystal_F_000 656
_exptl_absorpt_coefficient_mu 1.831
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_correction_T_min 0.54
_exptl_absorpt_correction_T_max 0.74
_exptl_absorpt_process_details
;
BRUKER AXS SMART APEX 2 Vers. 3.0-2009
R.H. Blessing, Acta Cryst. (1995) A51 33-38
;
_exptl_special_details
;
The crystallization was performed on the diffractometer at a temperature of
215 K with a miniature zone melting procedure using focussed infrared-laser-
radiation according to: R. Boese, M. Nussbaumer, "In Situ Crystallisation
Techniques", in: "Organic Crystal Chemistry",
Ed. D.W. Jones, Oxford University Press, Oxford, England, (1994) 20-37
;
# EXPERIMENTAL DATA
_diffrn_ambient_temperature 215(1)
_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
;
Siemens SMART three axis goniometer with APEX II area detector system
;
_diffrn_measurement_method
;
Data collection strategy APEX 2 / COSMO
with chi = 0 deg, phi +/- 10 deg
;
_diffrn_detector_area_resol_mean 512
_diffrn_standards_number ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time ?
_diffrn_standards_decay_% ?
_diffrn_reflns_number 4746
_diffrn_reflns_av_R_equivalents 0.0159
_diffrn_reflns_av_sigmaI/netI 0.0229
_diffrn_reflns_limit_h_min -8
_diffrn_reflns_limit_h_max 7
_diffrn_reflns_limit_k_min -8
_diffrn_reflns_limit_k_max 14
_diffrn_reflns_limit_l_min -17
_diffrn_reflns_limit_l_max 17
_diffrn_reflns_theta_min 2.51
_diffrn_reflns_theta_max 28.42
_reflns_number_total 2372
_reflns_number_gt 2243
_reflns_threshold_expression >2sigma(I)
_computing_data_collection 'BRUKER AXS SMART APEX 2 Vers. 3.0-2009'
_computing_cell_refinement 'BRUKER AXS SMART APEX 2 Vers. 3.0-2009'
_computing_data_reduction 'BRUKER AXS SMART APEX 2 Vers. 3.0-2009'
_computing_structure_solution 'BRUKER AXS SMART APEX 2 Vers. 3.0-2009'
_computing_structure_refinement 'BRUKER AXS SHELXTL (c) 2008 / Vers. 2008/4'
_computing_molecular_graphics 'BRUKER AXS SHELXTL (c) 2008 / Vers. 2008/4'
_computing_publication_material 'BRUKER AXS SHELXTL (c) 2008 / Vers. 2008/4'
# 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.
Treatment of hydrogen atoms
Riding model on idealized geometrics
with the 1.2 fold isotropic displacement
parameters of the equivalent Uij of the
corresponding carbon atom
;
_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^)+(0.0189P)^2^+0.8190P] 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 constr
_refine_ls_extinction_method SHELXL
_refine_ls_extinction_coef ?
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack 0.04(15)
_chemical_absolute_configuration ad
_refine_ls_number_reflns 2372
_refine_ls_number_parameters 111
_refine_ls_number_restraints 0
_refine_ls_R_factor_all 0.0298
_refine_ls_R_factor_gt 0.0273
_refine_ls_wR_factor_ref 0.0656
_refine_ls_wR_factor_gt 0.0640
_refine_ls_goodness_of_fit_ref 1.039
_refine_ls_restrained_S_all 1.039
_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 0.70407(12) 0.05377(9) 0.00785(6) 0.0623(3) Uani 1 1 d . . .
Cl2 Cl 0.91505(12) 0.25257(7) 0.07333(7) 0.0612(3) Uani 1 1 d . . .
Cl3 Cl 0.81137(11) 0.19718(8) 0.31118(5) 0.0571(2) Uani 1 1 d . . .
Cl4 Cl 0.92729(11) -0.02205(7) 0.19928(6) 0.0524(2) Uani 1 1 d . . .
Cl5 Cl 0.41847(12) 0.00788(8) 0.41256(7) 0.0651(3) Uani 1 1 d . . .
Cl6 Cl 0.17003(12) 0.18287(9) 0.45959(5) 0.0593(3) Uani 1 1 d . . .
Cl7 Cl 0.41267(11) 0.27494(7) 0.28012(8) 0.0637(3) Uani 1 1 d . . .
Cl8 Cl 0.33333(12) 0.04459(9) 0.16682(6) 0.0587(2) Uani 1 1 d . . .
C1 C 0.7535(4) 0.1619(3) 0.1081(2) 0.0434(8) Uani 1 1 d . . .
H1 H 0.6709 0.2196 0.1176 0.052 Uiso 1 1 d R . .
C2 C 0.7772(4) 0.0891(2) 0.2077(2) 0.0381(7) Uani 1 1 d . . .
H2 H 0.6866 0.0433 0.2233 0.046 Uiso 1 1 d R . .
C3 C 0.2509(4) 0.0796(3) 0.3649(2) 0.0424(7) Uani 1 1 d . . .
H3 H 0.1796 0.0133 0.3507 0.051 Uiso 1 1 d R . .
C4 C 0.2767(4) 0.1536(3) 0.2658(2) 0.0408(7) Uani 1 1 d . . .
H4 H 0.1834 0.1918 0.2450 0.049 Uiso 1 1 d 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 0.0613(7) 0.0764(5) 0.0492(4) -0.0214(4) -0.0141(4) 0.0158(5)
Cl2 0.0732(7) 0.0471(4) 0.0632(4) 0.0073(3) 0.0250(4) -0.0039(4)
Cl3 0.0585(7) 0.0684(5) 0.0442(3) -0.0178(3) 0.0031(4) -0.0052(4)
Cl4 0.0429(6) 0.0433(3) 0.0709(4) 0.0005(3) -0.0121(4) 0.0082(3)
Cl5 0.0662(7) 0.0643(5) 0.0649(5) 0.0145(4) -0.0189(5) 0.0200(5)
Cl6 0.0691(7) 0.0699(5) 0.0388(3) -0.0058(3) 0.0027(4) 0.0119(5)
Cl7 0.0470(7) 0.0389(3) 0.1052(7) 0.0049(4) 0.0110(5) -0.0068(4)
Cl8 0.0639(7) 0.0666(5) 0.0457(4) -0.0122(3) 0.0072(4) 0.0045(4)
C1 0.044(2) 0.0437(15) 0.0428(13) -0.0024(11) 0.0035(13) 0.0094(13)
C2 0.031(2) 0.0395(13) 0.0436(13) -0.0036(11) -0.0004(12) -0.0020(11)
C3 0.045(2) 0.0415(14) 0.0410(13) 0.0038(11) -0.0061(12) 0.0007(12)
C4 0.039(2) 0.0414(14) 0.0417(13) 0.0056(11) 0.0011(12) 0.0033(12)
# 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 1.771(3) . ?
Cl2 C1 1.777(3) . ?
Cl3 C2 1.774(3) . ?
Cl4 C2 1.774(3) . ?
Cl5 C3 1.775(3) . ?
Cl6 C3 1.780(3) . ?
Cl7 C4 1.763(3) . ?
Cl8 C4 1.782(3) . ?
C1 C2 1.504(4) . ?
C3 C4 1.508(4) . ?
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 109.02(19) . . ?
C2 C1 Cl2 111.9(2) . . ?
Cl1 C1 Cl2 111.14(16) . . ?
C1 C2 Cl3 109.59(19) . . ?
C1 C2 Cl4 112.8(2) . . ?
Cl3 C2 Cl4 109.76(16) . . ?
C4 C3 Cl5 112.5(2) . . ?
C4 C3 Cl6 108.88(19) . . ?
Cl5 C3 Cl6 111.12(15) . . ?
C3 C4 Cl7 112.8(2) . . ?
C3 C4 Cl8 108.23(19) . . ?
Cl7 C4 Cl8 110.23(17) . . ?
_diffrn_measured_fraction_theta_max 0.800
_diffrn_reflns_theta_full 28.42
_diffrn_measured_fraction_theta_full 0.800
_refine_diff_density_max 0.386
_refine_diff_density_min -0.260
_refine_diff_density_rms 0.045
_vrf_PLAT029_tcexdb0
;
PROBLEM: _diffrn_measured_fraction_theta_full Low ....... 0.80
RESPONSE:
The compounds are liquids at RT. The single crystals
are formed by an in-situ zone melting process inside a quartz capillary
using an IR-laser. The experimental setup does only allow for a
omega scan of the single crystal. This limits the completeness
to 75% to 95% depending on the crystal system.
;
_vrf_REFLT03_tcexdb0
;
PROBLEM: Completeness (_total/calc) 137.11%
RESPONSE:
Refinement as racemic twinning with matrix -1 0 0 0 -1 0 0 0 -1 2
with Flack absolute structure parameter 0.04(15) in the final structure
factor calculation
;
_vrf_PLAT950_tcexdb0
;
PROBLEM: _diffrn_measured_fraction_theta_full Low ....... 0.75
RESPONSE:
The compounds are liquids at RT. The single crystals
are formed by an in-situ zone melting process inside
a quartz capillaryusing an IR-laser.
The experimental setup does only allow for a
omega scan of the single crystal.
The range of +/-h, +/-k and +/-l depending on the
crystal system.
;
#############################################################################
data_1122TCE_065GPa
_database_code_depnum_ccdc_archive 'CCDC 811782'
#TrackingRef '- 1122TCELThp.cif'
# CHEMICAL DATA
_audit_update_record
;
2010-10-30 # Formatted by publCIF
;
_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 6.1941(9)
_cell_length_b 6.186(2)
_cell_length_c 7.361(3)
_cell_angle_alpha 90.00
_cell_angle_beta 104.90(2)
_cell_angle_gamma 90.00
_cell_volume 272.57(15)
_cell_formula_units_Z 2
_cell_measurement_temperature 295(2)
_cell_measurement_pressure 650000
_cell_measurement_reflns_used 2619
_cell_measurement_theta_min 3.39
_cell_measurement_theta_max 28.57
_exptl_crystal_description cylindric
_exptl_crystal_colour colorless
_exptl_crystal_size_max 0.48
_exptl_crystal_size_mid 0.48
_exptl_crystal_size_min 0.22
_exptl_crystal_density_meas ?
_exptl_crystal_density_diffrn 2.045
_exptl_crystal_density_method 'not measured'
_exptl_crystal_F_000 164
_exptl_absorpt_coefficient_mu 2.008
_exptl_absorpt_correction_type numerical
_exptl_absorpt_correction_T_min 0.218
_exptl_absorpt_correction_T_max 0.570
_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 0.65(5) GPa
(650000 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 650000
_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_% ?
_diffrn_reflns_number 1157
_diffrn_reflns_av_R_equivalents 0.1028
_diffrn_reflns_av_sigmaI/netI 0.0464
_diffrn_reflns_limit_h_min -7
_diffrn_reflns_limit_h_max 7
_diffrn_reflns_limit_k_min -5
_diffrn_reflns_limit_k_max 5
_diffrn_reflns_limit_l_min -7
_diffrn_reflns_limit_l_max 7
_diffrn_reflns_theta_min 3.40
_diffrn_reflns_theta_max 25.34
_reflns_number_total 198
_reflns_number_gt 191
_reflns_threshold_expression I>2\s(I)
_computing_data_collection 'CrysAlisCCD (Oxford Diffraction, 2004)'
_computing_cell_refinement 'CrysAlisRED (Oxford Diffraction, 2004)'
_computing_data_reduction
'CrysAlisRED (Oxford Diffraction, 2004); 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\^)+(0.0600P)\^2\^+0.8610P] 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 198
_refine_ls_number_parameters 31
_refine_ls_number_restraints 2
_refine_ls_R_factor_all 0.0620
_refine_ls_R_factor_gt 0.0598
_refine_ls_wR_factor_ref 0.1469
_refine_ls_wR_factor_gt 0.1435
_refine_ls_goodness_of_fit_ref 1.174
_refine_ls_restrained_S_all 1.170
_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_symetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.8851(14) 0.4797(16) 1.0174(15) 0.050(2) Uani 1 1 d D . .
H1 H 0.882(14) 0.514(11) 1.139(13) 0.060 Uiso 1 1 d D . .
Cl1 Cl 0.8093(3) 0.2067(4) 0.9869(3) 0.0519(9) Uani 1 1 d D . .
Cl2 Cl 0.6846(3) 0.6431(4) 0.8564(3) 0.0596(10) Uani 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
C1 0.055(4) 0.046(11) 0.048(9) 0.004(3) 0.013(4) 0.012(5)
Cl1 0.0526(13) 0.051(3) 0.049(3) -0.0003(7) 0.0070(12) -0.0039(9)
Cl2 0.0467(12) 0.070(3) 0.056(3) 0.0123(10) 0.0029(12) 0.0131(11)
# 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
C1 C1 1.531(17) 3_767 ?
C1 Cl1 1.751(11) . ?
C1 Cl2 1.792(10) . ?
C1 H1 0.93(9) . ?
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
C1 C1 Cl1 111.5(9) 3_767 . ?
C1 C1 Cl2 108.2(9) 3_767 . ?
Cl1 C1 Cl2 110.0(6) . . ?
C1 C1 H1 112(6) 3_767 . ?
Cl1 C1 H1 106(4) . . ?
Cl2 C1 H1 109(4) . . ?
_diffrn_measured_fraction_theta_max 0.394
_diffrn_reflns_theta_full 25.34
_diffrn_measured_fraction_theta_full 0.394
_refine_diff_density_max 0.280
_refine_diff_density_min -0.245
_refine_diff_density_rms 0.071
_vrf_REFLT03_1122TCE_065GPa
;
PROBLEM: Reflection count < 85% complete (theta max?)
RESPONSE:
All the Alerts generated below are the 'typical high-pressure crystallography
warnings'.
1,1,2,2-Tetrachloroethane (1122TCE) is a liquid at ambient conditions.
A single crystal of 1122TCE was obtained by the in-situ high-pressure
crystallization technique in a diamond-anvil cell (DAC).
The DAC imposes severe restrictions on which reflections can be collected,
resulting in a low data:parameter ratio and, in consequence, in a low-bond
precision.
The number of reflections depends on the crystal system and a single-crystal
orientation in a DAC.
;
_vrf_PLAT022_1122TCE_065GPa
;
PROBLEM: Ratio Unique / Expected Reflections too Low .... 0.39
RESPONSE:
1,1,2,2-Tetrachloroethane (1122TCE) is a liquid at ambient conditions.
A single crystal of 1122TCE was obtained by the in-situ high-pressure
crystallization technique in a diamond-anvil cell (DAC).
The DAC imposes severe restrictions on which reflections can be collected,
resulting in a low data:parameter ratio and, in consequence, in a low-bond
precision.
The number of reflections depends on the crystal system and a single-crystal
orientation in a DAC.
;
_vrf_PLAT029_1122TCE_065GPa
;
PROBLEM: _diffrn_measured_fraction_theta_full Low ....... 0.39
RESPONSE:
1,1,2,2-Tetrachloroethane (1122TCE) is a liquid at ambient conditions.
A single crystal of 1122TCE was obtained by the in-situ high-pressure
crystallization technique in a diamond-anvil cell (DAC).
The DAC imposes severe restrictions on which reflections can be collected,
resulting in a low data:parameter ratio and, in consequence, in a low-bond
precision.
The number of reflections depends on the crystal system and a single-crystal
orientation in a DAC.
;
_vrf_PLAT088_1122TCE_065GPa
;
PROBLEM: Poor Data / Parameter Ratio .................... 6.39
RESPONSE:
1,1,2,2-Tetrachloroethane (1122TCE) is a liquid at ambient conditions.
A single crystal of 1122TCE was obtained by the in-situ high-pressure
crystallization technique in a diamond-anvil cell (DAC).
The DAC imposes severe restrictions on which reflections can be collected,
resulting in a low data:parameter ratio and, in consequence, in a low-bond
precision.
The number of reflections depends on the crystal system and a single-crystal
orientation in a DAC.
;
_vrf_PLAT340_1122TCE_065GPa
;
PROBLEM: Low Bond Precision on C-C Bonds (x 1000) Ang .. 13
RESPONSE:
1,1,2,2-Tetrachloroethane (1122TCE) is a liquid at ambient conditions.
A single crystal of 1122TCE was obtained by the in-situ high-pressure
crystallization technique in a diamond-anvil cell (DAC).
The DAC imposes severe restrictions on which reflections can be collected,
resulting in a low data:parameter ratio and, in consequence, in a low-bond
precision.
The number of reflections depends on the crystal system and a single-crystal
orientation in a DAC.
;
_vrf_PLAT951_1122TCE_065GPa
;
PROBLEM: Reported and Calculated Kmax Values Differ by .. 2
RESPONSE:
1,1,2,2-Tetrachloroethane (1122TCE) is a liquid at ambient conditions.
A single crystal of 1122TCE was obtained by the in-situ high-pressure
crystallization technique in a diamond-anvil cell (DAC).
The DAC imposes severe restrictions on which reflections can be collected,
resulting in a low data:parameter ratio and, in consequence, in a low-bond
precision.
The number of reflections depends on the crystal system and a single-crystal
orientation in a DAC.
;
_vrf_PLAT860_1122TCE_065GPa
;
PROBLEM: Note: Number of Least-Squares Restraints ....... 2
RESPONSE:
The geometrical restraints were used for the hydrogen-atom
refinement.
;
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