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_4502812
_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 Cl3 O3, 2(C8 H10)'
_chemical_formula_sum            'C49 H53 Cl3 O3'
_chemical_formula_weight         796.3
_chemical_name_common            '1Cl. p-xylene'
_chemical_name_systematic
;
 1,3,5-triethyl-2,4,6-tris(4-chlorophenoxy)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                64.153(9)
_cell_angle_beta                 71.764(9)
_cell_angle_gamma                77.321(8)
_cell_formula_units_Z            2
_cell_length_a                   10.4401(10)
_cell_length_b                   15.6190(13)
_cell_length_c                   16.1505(15)
_cell_measurement_reflns_used    2755
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      29.2697
_cell_measurement_theta_min      2.6335
_cell_volume                     2240.4(4)
_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 0.998
_diffrn_measured_fraction_theta_max 0.846
_diffrn_measurement_details
;
  1 omega  -75.00  -48.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.1835  179.0000  150.0000 27

  2 omega   -9.00   30.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       18.9022   77.0000  -30.0000 39

  3 omega   30.00   67.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       18.9022 -112.0000    5.0000 37

  4 omega  -50.00    7.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       18.9022  -77.0000   90.0000 57

  5 omega  -11.00   89.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       18.9022   77.0000  120.0000 100

  6 omega  -13.00   13.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       18.9022 -112.0000    5.0000 26

  7 omega   43.00   84.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       18.9022   77.0000  -30.0000 41

  8 omega   44.00   95.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       18.9022  179.0000   90.0000 51

  9 omega  -51.00   49.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       18.9022  -77.0000 -150.0000 100
;
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0108079000
_diffrn_orient_matrix_UB_12      -0.0238710000
_diffrn_orient_matrix_UB_13      -0.0305913000
_diffrn_orient_matrix_UB_21      -0.0043975000
_diffrn_orient_matrix_UB_22      0.0447070000
_diffrn_orient_matrix_UB_23      -0.0386460000
_diffrn_orient_matrix_UB_31      0.0709195000
_diffrn_orient_matrix_UB_32      0.0014177000
_diffrn_orient_matrix_UB_33      -0.0103642000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.1108
_diffrn_reflns_av_unetI/netI     0.4228
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            21970
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         29.33
_diffrn_reflns_theta_min         2.64
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.244
_exptl_absorpt_correction_T_max  0.959
_exptl_absorpt_correction_T_min  0.946
_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    1.180
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             844
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.17
_refine_diff_density_max         0.169
_refine_diff_density_min         -0.215
_refine_diff_density_rms         0.037
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.737
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     503
_refine_ls_number_reflns         12300
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.737
_refine_ls_R_factor_all          0.3468
_refine_ls_R_factor_gt           0.0619
_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^)+(0.0315P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0825
_refine_ls_wR_factor_ref         0.1257
_reflns_number_gt                2108
_reflns_number_total             12300
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg2009144_si_001.cif
_cod_data_source_block           1Cl.p-xylene
_cod_database_code               4502812