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_7117273
_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 I3'
_chemical_formula_sum            'C9 H9 I3'
_chemical_formula_weight         497.86
_chemical_name_systematic
;
triiodomesitylene   
;
_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             2013-08-18
_audit_creation_method
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  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                60.183(6)
_cell_angle_beta                 66.729(6)
_cell_angle_gamma                85.377(5)
_cell_formula_units_Z            2
_cell_length_a                   8.0247(5)
_cell_length_b                   9.6025(5)
_cell_length_c                   9.6148(5)
_cell_measurement_reflns_used    2271
_cell_measurement_temperature    262(2)
_cell_measurement_theta_max      28.9904
_cell_measurement_theta_min      4.2929
_cell_volume                     584.24(8)
_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
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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      262(2)
_diffrn_detector_area_resol_mean 15.9821
_diffrn_measured_fraction_theta_full 0.9932
_diffrn_measured_fraction_theta_max 0.9364
_diffrn_measurement_details
;
  1 omega  -88.00    5.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -      -17.4178  -77.0000 -120.0000 93

  2 omega  -23.00   22.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -      -17.4178  -99.0000  120.0000 45

  3 omega  -77.00  -32.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -      -17.4178  178.0000   90.0000 45

  4 omega   42.00   88.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -       19.1366   57.0000  120.0000 46

  5 omega   35.00   91.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -       19.1366  178.0000  150.0000 56

  6 omega  -49.00   40.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -       19.1366  -57.0000  -30.0000 89

  7 omega  -88.00   13.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -      -17.4178  -77.0000    0.0000 101
;
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0531388000
_diffrn_orient_matrix_UB_12      0.0777952000
_diffrn_orient_matrix_UB_13      -0.0621976000
_diffrn_orient_matrix_UB_21      0.0400881000
_diffrn_orient_matrix_UB_22      -0.0248798000
_diffrn_orient_matrix_UB_23      -0.0628331000
_diffrn_orient_matrix_UB_31      -0.0708999000
_diffrn_orient_matrix_UB_32      0.0270844000
_diffrn_orient_matrix_UB_33      -0.0296384000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0251
_diffrn_reflns_av_unetI/netI     0.0351
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            5409
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         29.05
_diffrn_reflns_theta_min         4.30
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    7.976
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.52196
_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    2.830
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             444
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.3
_refine_diff_density_max         0.707
_refine_diff_density_min         -1.091
_refine_diff_density_rms         0.167
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     112
_refine_ls_number_reflns         2649
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.0386
_refine_ls_R_factor_gt           0.0301
_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^)+(0.0288P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0643
_refine_ls_wR_factor_ref         0.0681
_reflns_number_gt                2237
_reflns_number_total             2649
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5cc03033a2.cif
_cod_data_source_block           tim-262K
_cod_original_cell_volume        584.24(6)
_cod_database_code               7117273