Evolution of intermolecular contacts with temperature and pressure in bromoethane and iodoethane – a comparative study
Bujak, Maciej; Olejniczak, Anna; Podsiadło, Marcin; Acta Crystallographica Section B 78 (2022) –; doi:10.1107/S2052520622010149

data_2109087
_publ_section_title
;
 Evolution of intermolecular contacts with temperature and pressure in
 bromoethane and iodoethane -- a comparative study
;
_journal_coeditor_code           AW5073
_journal_issue                   6
_journal_name_full               'Acta Crystallographica Section B'
_journal_page_first
;
;
_journal_paper_doi               10.1107/S2052520622010149
_journal_volume                  78
_journal_year                    2022
_chemical_formula_moiety         'C2 H5 I'
_chemical_formula_sum            'C2 H5 I'
_chemical_formula_weight         155.96
_chemical_name_systematic        iodoethane
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2018/3
_cell_angle_alpha                90
_cell_angle_beta                 102.262(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   5.5767(13)
_cell_length_b                   9.7073(6)
_cell_length_c                   6.8424(3)
_cell_measurement_reflns_used    1135
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      26.72
_cell_measurement_theta_min      4.76
_cell_volume                     361.96(9)
_computing_cell_refinement
'CrysAlisPro 1.171.40.84a (Rigaku Oxford Diffraction, 2020)'
_computing_data_collection
'CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)'
_computing_data_reduction
'CrysAlisPro 1.171.40.84a (Rigaku Oxford Diffraction, 2020)'
_computing_molecular_graphics    'Mercury (Macrae at al., 2020)'
_computing_publication_material  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXS-2013/1 (Sheldrick, 2013)'
_diffrn_ambient_environment      'diamond-anvil cell'
_diffrn_ambient_pressure         1880000
_diffrn_ambient_temperature      295(2)
_diffrn_measured_fraction_theta_full 0.424
_diffrn_measured_fraction_theta_max 0.386
_diffrn_measurement_device_type  'KUMA KM4-CCD, Eos'
_diffrn_measurement_method       '\f- and \w-scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0254
_diffrn_reflns_av_unetI/netI     0.0124
_diffrn_reflns_Laue_measured_fraction_full 0.424
_diffrn_reflns_Laue_measured_fraction_max 0.386
_diffrn_reflns_limit_h_max       4
_diffrn_reflns_limit_h_min       -4
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            1671
_diffrn_reflns_point_group_measured_fraction_full 0.424
_diffrn_reflns_point_group_measured_fraction_max 0.386
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.772
_diffrn_reflns_theta_min         4.780
_exptl_absorpt_coefficient_mu    8.571
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.118
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.84a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.862
_exptl_crystal_description       disc
_exptl_crystal_F_000             280
_exptl_crystal_size_max          0.37
_exptl_crystal_size_mid          0.37
_exptl_crystal_size_min          0.21
_refine_diff_density_max         0.474
_refine_diff_density_min         -0.412
_refine_diff_density_rms         0.124
_refine_ls_extinction_coef       0.172(12)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.256
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     30
_refine_ls_number_reflns         299
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.247
_refine_ls_R_factor_all          0.0268
_refine_ls_R_factor_gt           0.0256
_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^)+(0.0437P)^2^+0.2787P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0682
_refine_ls_wR_factor_ref         0.0685
_reflns_Friedel_coverage         0.000
_reflns_number_gt                293
_reflns_number_total             299
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            aw5073sup1.cif
_cod_data_source_block           MIE_1.88GPa
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               2109087
_publcif_datablock.id            {1ce1679f-83cf-4728-ab0e-ec0ee29f00b2}
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.144
_shelx_estimated_absorpt_t_max   0.266
_exptl_absorpt_special_details
;
Data were collected at room temperature (295(2) K) and pressure of 1.88(2) GPa
(1880000 kPa).
;
_shelx_res_checksum              38771
_shelx_hkl_checksum              46717
_cod_database_fobs_code 2109087