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_7117271
_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             2013-09-29
_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                60.223(6)
_cell_angle_beta                 66.693(6)
_cell_angle_gamma                85.452(5)
_cell_formula_units_Z            2
_cell_length_a                   7.9700(5)
_cell_length_b                   9.5781(6)
_cell_length_c                   9.5874(6)
_cell_measurement_reflns_used    2392
_cell_measurement_temperature    190(2)
_cell_measurement_theta_max      29.0990
_cell_measurement_theta_min      4.4385
_cell_volume                     577.07(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
;
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      190(2)
_diffrn_detector_area_resol_mean 15.9821
_diffrn_measured_fraction_theta_full 0.9932
_diffrn_measured_fraction_theta_max 0.9356
_diffrn_measurement_details
;
  1 omega  -25.00   22.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -      -17.4178  -99.0000 -150.0000 47

  2 omega  -65.00  -38.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -      -17.4178 -178.0000  -90.0000 27

  3 omega  -22.00   16.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -       19.1366   99.0000   35.0000 38

  4 omega   -4.00   89.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -       19.1366   37.0000 -150.0000 93

  5 omega    1.00   86.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -       19.1366   57.0000  -60.0000 85

  6 omega  -48.00   45.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -       19.1366  -37.0000   30.0000 93

  7 omega  -94.00  -32.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -      -17.4178  178.0000  120.0000 62

  8 omega   -2.00   37.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -       19.1366   57.0000   60.0000 39
;
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0535762000
_diffrn_orient_matrix_UB_12      0.0780175000
_diffrn_orient_matrix_UB_13      -0.0624398000
_diffrn_orient_matrix_UB_21      0.0402145000
_diffrn_orient_matrix_UB_22      -0.0248951000
_diffrn_orient_matrix_UB_23      -0.0630835000
_diffrn_orient_matrix_UB_31      -0.0714845000
_diffrn_orient_matrix_UB_32      0.0270879000
_diffrn_orient_matrix_UB_33      -0.0295033000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0269
_diffrn_reflns_av_unetI/netI     0.0379
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            5479
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         29.16
_diffrn_reflns_theta_min         4.45
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    8.075
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.41945
_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    2.865
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             444
_exptl_crystal_size_max          0.44
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.3
_refine_diff_density_max         0.783
_refine_diff_density_min         -1.274
_refine_diff_density_rms         0.184
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.088
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     112
_refine_ls_number_reflns         2653
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.088
_refine_ls_R_factor_all          0.0374
_refine_ls_R_factor_gt           0.0312
_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^)+(0.0294P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0672
_refine_ls_wR_factor_ref         0.0698
_reflns_number_gt                2339
_reflns_number_total             2653
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5cc03033a2.cif
_cod_data_source_block           tim-190K
_cod_original_cell_volume        577.07(6)
_cod_database_code               7117271