A thermal expansion investigation of the melting point anomaly in trihalomesitylenes
Viswanadha G. Saraswatula; Binoy K. Saha; Chem.Commun. 51 (2015) 9829–; doi:10.1039/C5cc03033A

data_7117262
_publ_section_title
;
 A thermal expansion investigation of the melting point anomaly in
 trihalomesitylenes
;
_journal_name_full               Chem.Commun.
_journal_page_first              9829
_journal_paper_doi               10.1039/C5cc03033A
_journal_volume                  51
_journal_year                    2015
_chemical_formula_moiety         'C9 H9 Br3'
_chemical_formula_sum            'C9 H9 Br3'
_chemical_formula_weight         356.89
_chemical_name_systematic
;
tribromomesitylene 
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_audit_creation_date             2013-09-28
_audit_creation_method
;
  Olex2 1.2
  (compiled Dec  5 2012 16:17:34, GUI svn.r4385)
;
_audit_update_record
;
2015-04-06 deposited with the CCDC.
2015-05-07 downloaded from the CCDC.
;
_cell_angle_alpha                119.773(10)
_cell_angle_beta                 106.867(9)
_cell_angle_gamma                95.034(8)
_cell_formula_units_Z            2
_cell_length_a                   7.7305(7)
_cell_length_b                   9.0698(8)
_cell_length_c                   9.0855(9)
_cell_measurement_reflns_used    1388
_cell_measurement_temperature    226(2)
_cell_measurement_theta_max      29.0661
_cell_measurement_theta_min      4.1097
_cell_volume                     508.12(11)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET)
(compiled Sep 14 2012,17:21:16)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET)
(compiled Sep 14 2012,17:21:16)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET)
(compiled Sep 14 2012,17:21:16)
;
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement
;
SHELXL, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution
;
olex2.solve (L.J. Bourhis, O.V. Dolomanov, R.J. Gildea, J.A.K. Howard,
H. Puschmann, in preparation, 2011)
;
_diffrn_ambient_temperature      226(2)
_diffrn_detector_area_resol_mean 15.9821
_diffrn_measured_fraction_theta_full 0.9928
_diffrn_measured_fraction_theta_max 0.9327
_diffrn_measurement_details
;
  1 omega  -34.00   51.00   1.0000    4.5000
omega____ theta____ kappa____ phi______ frames
    -      -17.3397   57.0000    0.0000 85

  2 omega  -20.00   25.00   1.0000    4.5000
omega____ theta____ kappa____ phi______ frames
    -      -17.3397 -102.0000    7.0000 45

  3 omega  -32.00   46.00   1.0000    4.5000
omega____ theta____ kappa____ phi______ frames
    -      -17.3397   57.0000  120.0000 78

  4 omega  -23.00    3.00   1.0000    4.5000
omega____ theta____ kappa____ phi______ frames
    -      -17.3397  -99.0000  150.0000 26

  5 omega  -29.00   51.00   1.0000    4.5000
omega____ theta____ kappa____ phi______ frames
    -      -17.3397   57.0000 -120.0000 80

  6 omega   35.00   62.00   1.0000    4.5000
omega____ theta____ kappa____ phi______ frames
    -       19.0585  178.0000 -120.0000 27

  7 omega   32.00   61.00   1.0000    4.5000
omega____ theta____ kappa____ phi______ frames
    -       19.0585  -99.0000  -90.0000 29

  8 omega  -87.00   13.00   1.0000    4.5000
omega____ theta____ kappa____ phi______ frames
    -      -17.3397  -77.0000 -120.0000 100
;
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0503276000
_diffrn_orient_matrix_UB_12      0.0459088000
_diffrn_orient_matrix_UB_13      0.0541869000
_diffrn_orient_matrix_UB_21      0.0773922000
_diffrn_orient_matrix_UB_22      0.0771027000
_diffrn_orient_matrix_UB_23      0.0541417000
_diffrn_orient_matrix_UB_31      -0.0380347000
_diffrn_orient_matrix_UB_32      0.0274008000
_diffrn_orient_matrix_UB_33      -0.0603171000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0398
_diffrn_reflns_av_unetI/netI     0.0616
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            4728
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         29.13
_diffrn_reflns_theta_min         4.12
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    11.851
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.25114
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET)
(compiled Sep 14 2012,17:21:16)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.333
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             336
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.804
_refine_diff_density_min         -0.736
_refine_diff_density_rms         0.144
_refine_ls_extinction_coef       0.0204(12)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.013
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     113
_refine_ls_number_reflns         2329
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.013
_refine_ls_R_factor_all          0.0579
_refine_ls_R_factor_gt           0.0381
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0307P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0740
_refine_ls_wR_factor_ref         0.0827
_reflns_number_gt                1794
_reflns_number_total             2329
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5cc03033a2.cif
_cod_data_source_block           tbm-226K
_cod_original_cell_volume        508.12(8)
_cod_database_code               7117262