Relations between compression and thermal contraction in 1,2,4-trichlorobenzene and melting of trichlorobenzene isomers
Bujak, Maciej; Podsiadło, Marcin; Katrusiak, Andrzej; CrystEngComm 17 (2015) 3446–; doi:10.1039/C4CE02289K

data_7220022
_publ_section_title
;
 Relations between compression and thermal contraction in
 1,2,4-trichlorobenzene and melting of trichlorobenzene isomers
;
_journal_issue                   18
_journal_name_full               CrystEngComm
_journal_page_first              3446
_journal_paper_doi               10.1039/C4CE02289K
_journal_volume                  17
_journal_year                    2015
_chemical_formula_moiety         'C6 H3 Cl3'
_chemical_formula_sum            'C6 H3 Cl3'
_chemical_formula_weight         181.43
_chemical_melting_point          290.07
_chemical_name_systematic
; 
 1,2,4-trichlorobenzene 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2015-02-23 deposited with the CCDC.
2015-03-27 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 93.76(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   3.7825(7)
_cell_length_b                   26.378(3)
_cell_length_c                   13.71(4)
_cell_measurement_reflns_used    2420
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      29.34
_cell_measurement_theta_min      2.75
_cell_volume                     1365(4)
_computing_cell_refinement       'CrysAlisPro (Agilent Technologies, 2010)'
_computing_data_collection       'CrysAlisCCD (Oxford Diffraction, 2009)'
_computing_data_reduction
'CrysAlisPro (Agilent Technologies, 2010); REDSHABS (Katrusiak, A., 2003)'
_computing_molecular_graphics    'Mercury (Macrae at al., 2008)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_environment      'diamond-anvil cell'
_diffrn_ambient_pressure         640000
_diffrn_ambient_temperature      295(2)
_diffrn_detector_area_resol_mean 8.1929
_diffrn_measured_fraction_theta_full 0.219
_diffrn_measured_fraction_theta_max 0.219
_diffrn_measurement_device_type  'KUMA KM-4 CCD'
_diffrn_measurement_method       '\f- and \w-scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1388
_diffrn_reflns_av_sigmaI/netI    0.0472
_diffrn_reflns_limit_h_max       4
_diffrn_reflns_limit_h_min       -4
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       3
_diffrn_reflns_limit_l_min       -3
_diffrn_reflns_number            6941
_diffrn_reflns_theta_full        24.94
_diffrn_reflns_theta_max         24.94
_diffrn_reflns_theta_min         3.09
_exptl_absorpt_coefficient_mu    1.234
_exptl_absorpt_correction_T_max  0.72
_exptl_absorpt_correction_T_min  0.38
_exptl_absorpt_correction_type   numerical
_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).
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.766
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       disc
_exptl_crystal_F_000             720
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.24
_refine_diff_density_max         0.560
_refine_diff_density_min         -0.528
_refine_diff_density_rms         0.128
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.446
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     103
_refine_ls_number_reflns         528
_refine_ls_number_restraints     56
_refine_ls_restrained_S_all      1.423
_refine_ls_R_factor_all          0.1279
_refine_ls_R_factor_gt           0.1112
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
; 
 calc w=1/[\s\^2\^(Fo\^2\^)+(0.1876P)\^2\^+0.0000P] where
 P=(Fo\^2\^+2Fc\^2\^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2840
_refine_ls_wR_factor_ref         0.3072
_reflns_number_gt                434
_reflns_number_total             528
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4ce02289k2.cif
_cod_data_source_block           124TCB_0.64GPa
_cod_depositor_comments
'Adding full bibliography for 7220019--7220022.cif.'
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7220022