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_4502799
_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 Br3 O3, C8 H10'
_chemical_formula_sum            'C41 H43 Br3 O3'
_chemical_formula_weight         823.45
_chemical_name_common            '1Br, p-xylene'
_chemical_name_systematic
;
1,3,5-triethyl-2,4,6-tris(4-bromophenoxy)methylbenzene, p-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                70.52(2)
_cell_angle_beta                 83.247(19)
_cell_angle_gamma                89.667(18)
_cell_formula_units_Z            2
_cell_length_a                   9.808(2)
_cell_length_b                   13.395(3)
_cell_length_c                   15.310(4)
_cell_measurement_reflns_used    2551
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      29.3143
_cell_measurement_theta_min      2.6363
_cell_volume                     1881.9(8)
_computing_cell_refinement
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.66 (release 28-04-2010 CrysAlis171 .NET)
(compiled Apr 28 2010,14:27:37)
;
_computing_data_collection
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.66 (release 28-04-2010 CrysAlis171 .NET)
(compiled Apr 28 2010,14:27:37)
;
_computing_data_reduction
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.66 (release 28-04-2010 CrysAlis171 .NET)
(compiled Apr 28 2010,14:27:37)
;
_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 0.997
_diffrn_measured_fraction_theta_max 0.830
_diffrn_measurement_details
;
  1 omega  -83.00  -40.00   1.0000    7.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.4178  179.0000   60.0000 43

  2 omega  -20.00   22.00   1.0000    7.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.4178 -101.0000  -12.0000 42

  3 omega   25.00   57.00   1.0000    7.0000
omega____ theta____ kappa____ phi______ frames
    -       19.2147 -101.0000  167.0000 32

  4 omega   38.00   76.00   1.0000    7.0000
omega____ theta____ kappa____ phi______ frames
    -       19.2147  179.0000  -30.0000 38

  5 omega   15.00   60.00   1.0000    7.0000
omega____ theta____ kappa____ phi______ frames
    -       19.2147 -101.0000  -92.0000 45

  6 omega   65.00   92.00   1.0000    7.0000
omega____ theta____ kappa____ phi______ frames
    -       19.2147  179.0000  150.0000 27

  7 omega   -7.00   85.00   1.0000    7.0000
omega____ theta____ kappa____ phi______ frames
    -       19.2147   37.0000  120.0000 92

  8 omega  -53.00   45.00   1.0000    7.0000
omega____ theta____ kappa____ phi______ frames
    -       19.2147  -37.0000  -60.0000 98
;
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0535797753
_diffrn_orient_matrix_UB_12      -0.0252775397
_diffrn_orient_matrix_UB_13      0.0359045293
_diffrn_orient_matrix_UB_21      0.0280609915
_diffrn_orient_matrix_UB_22      0.0221419470
_diffrn_orient_matrix_UB_23      0.0303893441
_diffrn_orient_matrix_UB_31      -0.0406398018
_diffrn_orient_matrix_UB_32      0.0450363077
_diffrn_orient_matrix_UB_33      -0.0154666416
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0510
_diffrn_reflns_av_unetI/netI     0.1794
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            16119
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         29.38
_diffrn_reflns_theta_min         2.64
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    3.252
_exptl_absorpt_correction_T_max  0.594
_exptl_absorpt_correction_T_min  0.408
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.66 (release 28-04-2010 CrysAlis171 .NET)
(compiled Apr 28 2010,14:27:37)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.453
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             836
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.469
_refine_diff_density_min         -0.615
_refine_diff_density_rms         0.063
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.734
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     448
_refine_ls_number_reflns         8614
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.734
_refine_ls_R_factor_all          0.1529
_refine_ls_R_factor_gt           0.0440
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0425P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0839
_refine_ls_wR_factor_ref         0.0955
_reflns_number_gt                3049
_reflns_number_total             10377
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg2009144_si_001.cif
_cod_data_source_block           1Br.p-xylene
_cod_database_code               4502799