Five new Sb(V) bromide complexes and their polybromide derivatives with pyridinium-type cations: Structures, thermal stability and features of halogen⋯halogen contacts in solid state
Adonin, Sergey A.; Bondarenko, Mikhail A.; Novikov, Alexander S.; Plyusnin, Pavel E.; Korolkov, Ilya V.; Sokolov, Maxim N.; Fedin, Vladimir P.; Inorganica Chimica Acta 502 (2020) 119278–; doi:10.1016/j.ica.2019.119278

data_1565455
_publ_section_title
;
 Five new Sb(V) bromide complexes and their polybromide derivatives with
 pyridinium-type cations: Structures, thermal stability and features of
 halogen&#x22EF;halogen contacts in solid state
;
_journal_name_full               'Inorganica Chimica Acta'
_journal_page_first              119278
_journal_paper_doi               10.1016/j.ica.2019.119278
_journal_volume                  502
_journal_year                    2020
_chemical_formula_sum            'C16 H24 Br9 N2 Sb'
_chemical_formula_weight         1085.31
_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   geom
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 100.782(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   11.4927(4)
_cell_length_b                   7.3613(2)
_cell_length_c                   16.9266(6)
_cell_measurement_reflns_used    2603
_cell_measurement_temperature    130(2)
_cell_measurement_theta_max      28.5750
_cell_measurement_theta_min      3.6300
_cell_volume                     1406.73(8)
_computing_cell_refinement       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      130(2)
_diffrn_detector_area_resol_mean 10.6168
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.842
_diffrn_measurement_device_type  'New Xcalibur, AtlasS2'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0273
_diffrn_reflns_av_unetI/netI     0.0434
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.842
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            6398
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.842
_diffrn_reflns_theta_full        25.500
_diffrn_reflns_theta_max         28.874
_diffrn_reflns_theta_min         3.304
_diffrn_source                   'fine-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    13.771
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.45637
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    2.562
_exptl_crystal_description       block
_exptl_crystal_F_000             1000
_exptl_crystal_size_max          0.210
_exptl_crystal_size_mid          0.190
_exptl_crystal_size_min          0.100
_refine_diff_density_max         0.652
_refine_diff_density_min         -0.654
_refine_diff_density_rms         0.137
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.980
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     132
_refine_ls_number_reflns         3105
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.980
_refine_ls_R_factor_all          0.0409
_refine_ls_R_factor_gt           0.0278
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0118P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0452
_refine_ls_wR_factor_ref         0.0491
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2529
_reflns_number_total             3105
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ICA-2020-502-119278.cif
_cod_data_source_block           BM82_a
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               1565455
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.160
_shelx_estimated_absorpt_t_max   0.340
_shelx_res_checksum              41092
_shelx_hkl_checksum              21417