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_4502793
_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, C2 H4 Br2'
_chemical_formula_sum            'C35 H37 Br2 I3 O3'
_chemical_formula_weight         1046.17
_chemical_name_common            '1I, DBE'
_chemical_name_systematic
;
1,3,5-triethyl-2,4,6-tris(4-iodophenoxy)methylbenzene, 1,2-dibromoethane
;
_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                108.44(2)
_cell_angle_beta                 99.035(17)
_cell_angle_gamma                91.334(15)
_cell_formula_units_Z            2
_cell_length_a                   10.2538(16)
_cell_length_b                   13.144(3)
_cell_length_c                   15.119(4)
_cell_measurement_reflns_used    2115
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      29.2504
_cell_measurement_theta_min      2.6041
_cell_volume                     1903.3(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
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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
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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 0.996
_diffrn_measured_fraction_theta_max 0.831
_diffrn_measurement_details
;
  1 omega   35.00   62.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       18.9022  179.0000  -90.0000 27

  2 omega  -11.00   87.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       18.9022   77.0000   90.0000 98

  3 omega   -9.00   47.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       18.9022   77.0000 -150.0000 56

  4 omega  -45.00   46.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       18.9022  -77.0000  -30.0000 91

  5 omega   24.00   85.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       18.9022   77.0000 -120.0000 61

  6 omega  -51.00    5.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       18.9022  -77.0000   30.0000 56
;
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0682953638
_diffrn_orient_matrix_UB_12      -0.0159101111
_diffrn_orient_matrix_UB_13      -0.0061833963
_diffrn_orient_matrix_UB_21      -0.0125011385
_diffrn_orient_matrix_UB_22      0.0172041646
_diffrn_orient_matrix_UB_23      -0.0403170452
_diffrn_orient_matrix_UB_31      0.0107506247
_diffrn_orient_matrix_UB_32      -0.0520268682
_diffrn_orient_matrix_UB_33      -0.0292907787
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0974
_diffrn_reflns_av_unetI/netI     0.2118
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            15165
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         29.32
_diffrn_reflns_theta_min         2.61
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    4.594
_exptl_absorpt_correction_T_max  0.418
_exptl_absorpt_correction_T_min  0.309
_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    1.826
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1000
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.19
_refine_diff_density_max         1.073
_refine_diff_density_min         -0.943
_refine_diff_density_rms         0.147
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.828
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     381
_refine_ls_number_reflns         10417
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.828
_refine_ls_R_factor_all          0.2441
_refine_ls_R_factor_gt           0.0817
_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^)+(0.1178P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1940
_refine_ls_wR_factor_ref         0.2511
_reflns_number_gt                2532
_reflns_number_total             10417
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg2009144_si_001.cif
_cod_data_source_block           1I.DBE
_cod_original_cell_volume        1903.2(7)
_cod_database_code               4502793