Polymorphism and phase transformation in the dimethyl sulfoxide solvate of 2,3,5,6-tetrafluoro-1,4-diiodobenzene
Bond, Andrew D.; Truscott, Chris L.; Acta Crystallographica Section C 76 (2020) 524–529; doi:10.1107/S2053229620005690

data_2022105
_publ_section_title
;
 Polymorphism and phase transformation in the dimethyl sulfoxide solvate
 of 2,3,5,6-tetrafluoro-1,4-diiodobenzene
;
_journal_coeditor_code           SK3750
_journal_issue                   5
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              524
_journal_page_last               529
_journal_paper_doi               10.1107/S2053229620005690
_journal_volume                  76
_journal_year                    2020
_chemical_absolute_configuration ad
_chemical_formula_iupac          'C6 F4 I2, C2 H6 O S'
_chemical_formula_moiety         'C6 F4 I2, C2 H6 O S'
_chemical_formula_sum            'C8 H6 F4 I2 O S'
_chemical_formula_weight         479.99
_chemical_name_systematic
;
2,3,5,6-Tetrafluoro-1,4-diiodobenzene dimethyl sulfoxide
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab (x,y,z+1/4)'
_space_group_name_H-M_alt        'P 21 21 21 (origin shift x,y,z+1/4)'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2018/1
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.6731(2)
_cell_length_b                   18.0023(5)
_cell_length_c                   6.5470(2)
_cell_measurement_reflns_used    22578
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      1.02
_cell_volume                     1257.94(6)
_computing_cell_refinement
;
HKL SCALEPACK (Otwinowski & Minor, 1997)
;
_computing_data_collection
;
COLLECT (Nonius, 1998)
;
_computing_data_reduction
;
HKL DENZO and SCALEPACK (Otwinowski & Minor, 1997)
;
_computing_molecular_graphics
;
Mercury (Macrae <i>et al.</i>, 2020)
;
_computing_publication_material
;
SHELXL2018 (Sheldrick, 2015b)
;
_computing_structure_refinement
;
SHELXL2018 (Sheldrick, 2015b)
;
_computing_structure_solution
;
SHELXT (Sheldrick, 2015a)
;
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       '\w and \f-scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0887
_diffrn_reflns_av_unetI/netI     0.0888
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            11512
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.465
_diffrn_reflns_theta_min         3.651
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    5.191
_exptl_absorpt_correction_T_max  0.599
_exptl_absorpt_correction_T_min  0.475
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SORTAV; Blessing, 1995)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.534
_exptl_crystal_description       block
_exptl_crystal_F_000             880
_exptl_crystal_size_max          0.120
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.100
_refine_diff_density_max         0.913
_refine_diff_density_min         -1.175
_refine_ls_abs_structure_details 'Refined as an inversion twin.'
_refine_ls_abs_structure_Flack   0.19(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.990
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     148
_refine_ls_number_reflns         2834
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.990
_refine_ls_R_factor_all          0.0722
_refine_ls_R_factor_gt           0.0428
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0294P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0698
_refine_ls_wR_factor_ref         0.0775
_reflns_number_gt                2141
_reflns_number_total             2834
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            sk3750sup1.cif
_cod_data_source_block           Form_I_120K
_cod_original_cell_volume        1257.94(5)
_cod_original_sg_symbol_Hall     'P 2ac 2n'
_cod_original_sg_symbol_H-M      'P 21 21 21'
_cod_database_code               2022105
_cod_database_fobs_code          2022105
_shelx_estimated_absorpt_t_min   0.575
_shelx_estimated_absorpt_t_max   0.625
_shelx_hkl_checksum              4816
_shelx_res_checksum              41780