Rotationally disordered phase of 1,3-dibromo-5-iodo-2,4,6-trimethylbenzene at 293 K
Ghanemi, Soumia; Hernandez, Olivier; Boudjada, Ali; Meinnel, Jean; Acta Crystallographica Section C 65 (2009) o498–o501; doi:10.1107/S0108270109032715

data_2017328
_publ_section_title
;
 Rotationally disordered phase of
 1,3-dibromo-5-iodo-2,4,6-trimethylbenzene at 293 K
;
_journal_coeditor_code           FG3100
_journal_issue                   10
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              o498
_journal_page_last               o501
_journal_paper_doi               10.1107/S0108270109032715
_journal_volume                  65
_journal_year                    2009
_chemical_formula_iupac          'C9 H9 Br2 I'
_chemical_formula_moiety         'C9 H9 Br2 I'
_chemical_formula_sum            'C9 H9 Br2 I'
_chemical_formula_weight         403.84
_chemical_name_systematic
;
1,3-dibromo-5-iodo-2,4,6-trimethylbenzene
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_cell_angle_alpha                60.187(8)
_cell_angle_beta                 72.998(9)
_cell_angle_gamma                95.100(10)
_cell_formula_units_Z            2
_cell_length_a                   7.8950(10)
_cell_length_b                   9.3180(9)
_cell_length_c                   9.3130(11)
_cell_measurement_reflns_used    10298
_cell_measurement_temperature    293
_cell_measurement_theta_max      30.034
_cell_measurement_theta_min      2.91
_cell_volume                     545.33(13)
_computing_cell_refinement       'DIRAX (Duisenberg <i>et al.</i>,  2003)'
_computing_data_collection       'COLLECT (Nonius, 2001)'
_computing_data_reduction        'EvalCCD (Duisenberg <i>et al.</i>,  2003)'
_computing_molecular_graphics    'CAMERON (Watkin <i>et al.</i>,  1996)'
_computing_publication_material  'CRYSTALS (Betteridge <i>et al.</i>,  2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge <i>et al.</i>,  2003)'
_computing_structure_solution    'SIR97 (Altomare <i>et al.</i>,  1999)'
_diffrn_ambient_temperature      293.0(10)
_diffrn_measured_fraction_theta_full 0.978
_diffrn_measured_fraction_theta_max 0.942
_diffrn_measurement_device_type  'Nonius KappaCCD area-detector'
_diffrn_measurement_method       \w/2\q
_diffrn_radiation_monochromator  'horizontally mounted graphite crystal'
_diffrn_radiation_source         'X-ray tube'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.045
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            5479
_diffrn_reflns_theta_full        25.199
_diffrn_reflns_theta_max         29.999
_diffrn_reflns_theta_min         3.547
_exptl_absorpt_coefficient_mu    10.211
_exptl_absorpt_correction_T_max  0.16
_exptl_absorpt_correction_T_min  0.06
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.459
_exptl_crystal_description       plate
_exptl_crystal_F_000             371.964
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.18
_refine_diff_density_max         1.21
_refine_diff_density_min         -1.01
_refine_ls_extinction_coef       12(3)
_refine_ls_extinction_method     'Larson (1970), Eq. 22'
_refine_ls_goodness_of_fit_ref   1.1769
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     138
_refine_ls_number_reflns         1629
_refine_ls_number_restraints     54
_refine_ls_R_factor_all          0.0906
_refine_ls_R_factor_gt           0.0399
_refine_ls_shift/su_max          0.000206
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details
;
Method, part 1, Chebychev polynomial (Watkin, 1994, Prince, 1982)
[weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)],
where A~i~ are the Chebychev coefficients listed below and x = Fcalc/Fmax.
Method = Robust Weighting (Prince, 1982)
W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^
A~i~ are: 1.38 0.469 1.07
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0667
_refine_ls_wR_factor_ref         0.0436
_reflns_number_gt                1629
_reflns_number_total             2995
_reflns_threshold_expression     I>3\s(I)
_cod_data_source_file            fg3100.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               2017328
_cod_database_fobs_code          2017328