Halogen bonding in the structures of pentaiodobenzoic acid and its salts
Adonin, Sergey A.; Bondarenko, Mikhail A.; Novikov, Alexander S.; Abramov, Pavel A.; Sokolov, Maxim N.; Fedin, Vladimir P.; CrystEngComm 21 (2019) 6666–; doi:10.1039/C9CE01106D

data_7234933
_publ_section_title
;
 Halogen bonding in the structures of pentaiodobenzoic acid and its salts
;
_journal_issue                   43
_journal_name_full               CrystEngComm
_journal_page_first              6666
_journal_paper_doi               10.1039/C9CE01106D
_journal_volume                  21
_journal_year                    2019
_chemical_formula_sum            'C13 H16 I5 N O2'
_chemical_formula_weight         852.77
_space_group_crystal_system      orthorhombic
_space_group_IT_number           33
_space_group_name_Hall           'P 2c -2n'
_space_group_name_H-M_alt        'P n a 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2017/1
_audit_update_record
;
2019-05-29 deposited with the CCDC.	2019-09-24 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.9973(6)
_cell_length_b                   11.0540(5)
_cell_length_c                   10.3194(4)
_cell_measurement_reflns_used    6009
_cell_measurement_temperature    130(2)
_cell_measurement_theta_max      28.8680
_cell_measurement_theta_min      3.8220
_cell_volume                     2052.96(14)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_molecular_graphics    'ShelXle (H\"ubschle, 2011)'
_computing_publication_material  'CIFTAB-2014 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-2014 (Sheldrick, 2014)'
_diffrn_ambient_temperature      130(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.6168
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.919
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'New Xcalibur, AtlasS2'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0385
_diffrn_reflns_av_unetI/netI     0.0437
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.919
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            14763
_diffrn_reflns_point_group_measured_fraction_full 0.979
_diffrn_reflns_point_group_measured_fraction_max 0.846
_diffrn_reflns_theta_full        25.500
_diffrn_reflns_theta_max         29.007
_diffrn_reflns_theta_min         3.524
_diffrn_source                   'sealed X-ray tube'
_exptl_absorpt_coefficient_mu    7.578
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.66536
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.759
_exptl_crystal_description       block
_exptl_crystal_F_000             1528
_exptl_crystal_size_max          0.180
_exptl_crystal_size_mid          0.120
_exptl_crystal_size_min          0.060
_refine_diff_density_max         1.331
_refine_diff_density_min         -1.327
_refine_diff_density_rms         0.196
_refine_ls_abs_structure_details
;
 Flack x determined using 1709 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.03(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.107
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     193
_refine_ls_number_reflns         4615
_refine_ls_number_restraints     25
_refine_ls_restrained_S_all      1.105
_refine_ls_R_factor_all          0.0417
_refine_ls_R_factor_gt           0.0385
_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^)+(0.0342P)^2^+11.3404P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0856
_refine_ls_wR_factor_ref         0.0874
_reflns_Friedel_coverage         0.748
_reflns_Friedel_fraction_full    0.959
_reflns_Friedel_fraction_max     0.764
_reflns_number_gt                4352
_reflns_number_total             4615
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            c9ce01106d2.cif
_cod_data_source_block           SAC6I5COOHandEt3N_a
_cod_database_code               7234933
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_min   0.342
_shelx_estimated_absorpt_t_max   0.659
_shelx_res_checksum              13287