Isostructurality in the Guest Free Forms and in the Clathrates of 1,3,5-Triethyl-2,4,6-tris(4-halophenoxy)methylbenzenes
Bhattacharya, Suman; Saha, Binoy K.; Crystal Growth & Design 12 (2012) 169–; doi:10.1021/cg2009144

data_4502785
_publ_section_title
;
 Isostructurality in the Guest Free Forms and in the Clathrates of
 1,3,5-Triethyl-2,4,6-tris(4-halophenoxy)methylbenzenes
;
_journal_issue                   1
_journal_name_full               'Crystal Growth &amp; Design'
_journal_page_first              169
_journal_paper_doi               10.1021/cg2009144
_journal_volume                  12
_journal_year                    2012
_chemical_formula_moiety         'C33 H33 I3 O3, C8 H10'
_chemical_formula_sum            'C41 H43 I3 O3'
_chemical_formula_weight         964.45
_chemical_name_common            '1I, o-xylene'
_chemical_name_systematic
;
1,3,5-triethyl-2,4,6-tris(4-iodophenoxy)methylbenzenes, o-xylene
;
_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     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2011-09-21
_audit_creation_method
;
  Olex2 1.1
  (compiled 2011.08.18 svn.r1932, GUI svn.r3819)
;
_cell_angle_alpha                67.312(10)
_cell_angle_beta                 83.012(8)
_cell_angle_gamma                88.381(8)
_cell_formula_units_Z            2
_cell_length_a                   10.0282(9)
_cell_length_b                   13.4705(14)
_cell_length_c                   16.0032(17)
_cell_measurement_reflns_used    5473
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      29.2899
_cell_measurement_theta_min      2.6215
_cell_volume                     1979.3(4)
_computing_cell_refinement
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET)
(compiled Oct 25 2010,18:11:34)
;
_computing_data_collection
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET)
(compiled Oct 25 2010,18:11:34)
;
_computing_data_reduction
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET)
(compiled Oct 25 2010,18:11:34)
;
_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
;
XL, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      298(2)
_diffrn_detector_area_resol_mean 15.9821
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details
;
  1 omega  -21.00   24.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.4178 -102.0000  161.0000 45

  2 omega   -7.00   35.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.4178    0.0000   60.0000 42

  3 omega  -22.00    3.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.4178 -102.0000   95.0000 25

  4 omega  -89.00  -32.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.4178  179.0000  150.0000 57

  5 omega  -10.00   59.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       19.1366 -102.0000  -18.0000 69

  6 omega  -48.00   45.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       19.1366  -37.0000   90.0000 93

  7 omega   17.00   92.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       19.1366   37.0000   90.0000 75

  8 omega   -7.00   18.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       19.1366   37.0000  -60.0000 25
;
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0513969000
_diffrn_orient_matrix_UB_12      0.0151601000
_diffrn_orient_matrix_UB_13      -0.0374652000
_diffrn_orient_matrix_UB_21      -0.0403049000
_diffrn_orient_matrix_UB_22      0.0422458000
_diffrn_orient_matrix_UB_23      -0.0256834000
_diffrn_orient_matrix_UB_31      0.0285382000
_diffrn_orient_matrix_UB_32      0.0352763000
_diffrn_orient_matrix_UB_33      0.0166792000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0453
_diffrn_reflns_av_unetI/netI     0.0582
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            15049
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.63
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.403
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.51525
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET)
(compiled Oct 25 2010,18:11:34)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.618
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             944
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.18
_refine_diff_density_max         1.756
_refine_diff_density_min         -1.314
_refine_diff_density_rms         0.109
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     399
_refine_ls_number_reflns         6966
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.1004
_refine_ls_R_factor_gt           0.0661
_refine_ls_shift/su_max          1.799
_refine_ls_shift/su_mean         0.031
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1090P)^2^+2.0516P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1816
_refine_ls_wR_factor_ref         0.2123
_reflns_number_gt                4439
_reflns_number_total             6966
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg2009144_si_001.cif
_cod_data_source_block           1I.o-xylene
_cod_original_cell_volume        1979.3(3)
_cod_database_code               4502785