#------------------------------------------------------------------------------
#$Date: 2021-11-30 12:26:09 +0200 (Tue, 30 Nov 2021) $
#$Revision: 270940 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/56/54/1565453.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_1565453
loop_
_publ_author_name
'Adonin, Sergey A.'
'Bondarenko, Mikhail A.'
'Novikov, Alexander S.'
'Plyusnin, Pavel E.'
'Korolkov, Ilya V.'
'Sokolov, Maxim N.'
'Fedin, Vladimir P.'
_publ_section_title
;
 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
;
_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            'C7 H0 Br6 N Sb'
_chemical_formula_weight         699.29
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                75.226(4)
_cell_angle_beta                 88.079(4)
_cell_angle_gamma                79.872(4)
_cell_formula_units_Z            2
_cell_length_a                   7.6803(4)
_cell_length_b                   8.5900(4)
_cell_length_c                   12.6261(5)
_cell_measurement_reflns_used    1762
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      29.3990
_cell_measurement_theta_min      2.4920
_cell_volume                     792.84(7)
_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      150(2)
_diffrn_detector_area_resol_mean 10.6168
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.834
_diffrn_measurement_device_type  'New Xcalibur, AtlasS2'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0360
_diffrn_reflns_av_unetI/netI     0.0708
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.834
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            6073
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.834
_diffrn_reflns_theta_full        25.500
_diffrn_reflns_theta_max         29.465
_diffrn_reflns_theta_min         2.490
_diffrn_source                   'fine-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    16.831
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.20486
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    2.929
_exptl_crystal_description       block
_exptl_crystal_F_000             620
_exptl_crystal_size_max          0.320
_exptl_crystal_size_mid          0.160
_exptl_crystal_size_min          0.120
_refine_diff_density_max         3.040
_refine_diff_density_min         -2.225
_refine_diff_density_rms         0.361
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.933
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     136
_refine_ls_number_reflns         3675
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.933
_refine_ls_R_factor_all          0.0799
_refine_ls_R_factor_gt           0.0574
_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/[σ²(Fo²)+(0.1000P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1436
_refine_ls_wR_factor_ref         0.1655
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2653
_reflns_number_total             3675
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            ICA-2020-502-119278.cif
_cod_data_source_block           BM43_a
_cod_original_cell_volume        792.85(7)
_cod_database_code               1565453
_shelx_shelxl_version_number     2014/7
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_min   0.075
_shelx_estimated_absorpt_t_max   0.237
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Sb1 Sb 0.24747(7) 0.69570(6) 0.20917(4) 0.01930(18) Uani 1 1 d . . . . .
Br1 Br 0.46474(12) 0.77651(12) 0.05808(7) 0.0314(3) Uani 1 1 d . . . . .
C1 C 0.8041(12) 0.3897(11) 0.1562(8) 0.033(2) Uani 1 1 d . . . . .
H1A H 0.7879 0.3646 0.0861 0.050 Uiso 1 1 calc R U . . .
H1B H 0.9228 0.4152 0.1599 0.050 Uiso 1 1 calc R U . . .
H1C H 0.7155 0.4839 0.1626 0.050 Uiso 1 1 calc R U . . .
N1 N 0.7829(9) 0.2461(9) 0.2473(5) 0.0237(16) Uani 1 1 d . . . . .
Br2 Br 0.49972(13) 0.60058(12) 0.34984(7) 0.0322(3) Uani 1 1 d . . . . .
C2 C 0.8175(11) 0.2513(11) 0.3486(7) 0.0263(19) Uani 1 1 d . . . . .
H2 H 0.8561 0.3445 0.3610 0.032 Uiso 1 1 calc R U . . .
C3 C 0.7972(12) 0.1199(11) 0.4370(7) 0.030(2) Uani 1 1 d . . . . .
H3 H 0.8260 0.1230 0.5089 0.036 Uiso 1 1 calc R U . . .
Br3 Br 0.29048(12) 0.40742(11) 0.18071(7) 0.0282(2) Uani 1 1 d . . . . .
Br4 Br 0.03909(13) 0.61507(12) 0.36852(7) 0.0311(3) Uani 1 1 d . . . . .
C4 C 0.7366(11) -0.0128(11) 0.4214(7) 0.0263(19) Uani 1 1 d . . . . .
C5 C 0.7038(11) -0.0135(11) 0.3139(7) 0.027(2) Uani 1 1 d . . . . .
H5 H 0.6635 -0.1043 0.2990 0.033 Uiso 1 1 calc R U . . .
Br5 Br -0.01478(12) 0.78428(12) 0.07816(7) 0.0306(3) Uani 1 1 d . . . . .
C6 C 0.7296(11) 0.1175(11) 0.2286(7) 0.028(2) Uani 1 1 d . . . . .
H6 H 0.7087 0.1149 0.1553 0.034 Uiso 1 1 calc R U . . .
Br6 Br 0.21023(13) 0.98460(11) 0.23645(8) 0.0314(3) Uani 1 1 d . . . . .
C7 C 0.7096(13) -0.1515(13) 0.5141(8) 0.037(2) Uani 1 1 d . . . . .
H7A H 0.8237 -0.2054 0.5495 0.055 Uiso 1 1 calc R U . . .
H7B H 0.6569 -0.2300 0.4868 0.055 Uiso 1 1 calc R U . . .
H7C H 0.6303 -0.1110 0.5673 0.055 Uiso 1 1 calc R U . . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Sb Sb -0.5866 1.5461 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
Br5 Sb1 Br1 92.92(3) . .
Br5 Sb1 Br2 176.73(3) . .
Br1 Sb1 Br2 90.34(3) . .
Br5 Sb1 Br3 90.47(3) . .
Br1 Sb1 Br3 90.61(3) . .
Br2 Sb1 Br3 89.27(3) . .
Br5 Sb1 Br6 90.09(4) . .
Br1 Sb1 Br6 88.47(3) . .
Br2 Sb1 Br6 90.23(4) . .
Br3 Sb1 Br6 178.95(3) . .
Br5 Sb1 Br4 89.69(3) . .
Br1 Sb1 Br4 177.20(4) . .
Br2 Sb1 Br4 87.06(3) . .
Br3 Sb1 Br4 90.40(3) . .
Br6 Sb1 Br4 90.50(3) . .
N1 C1 H1A 109.5 . .
N1 C1 H1B 109.5 . .
H1A C1 H1B 109.5 . .
N1 C1 H1C 109.5 . .
H1A C1 H1C 109.5 . .
H1B C1 H1C 109.5 . .
C6 N1 C2 120.8(7) . .
C6 N1 C1 121.1(7) . .
C2 N1 C1 118.1(8) . .
N1 C2 C3 120.0(8) . .
N1 C2 H2 120.0 . .
C3 C2 H2 120.0 . .
C4 C3 C2 120.9(8) . .
C4 C3 H3 119.5 . .
C2 C3 H3 119.5 . .
C3 C4 C5 116.9(8) . .
C3 C4 C7 121.9(8) . .
C5 C4 C7 121.2(8) . .
C6 C5 C4 120.2(9) . .
C6 C5 H5 119.9 . .
C4 C5 H5 119.9 . .
N1 C6 C5 121.0(8) . .
N1 C6 H6 119.5 . .
C5 C6 H6 119.5 . .
C4 C7 H7A 109.5 . .
C4 C7 H7B 109.5 . .
H7A C7 H7B 109.5 . .
C4 C7 H7C 109.5 . .
H7A C7 H7C 109.5 . .
H7B C7 H7C 109.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Sb1 Br5 2.5327(10) .
Sb1 Br1 2.5346(9) .
Sb1 Br2 2.5513(10) .
Sb1 Br3 2.5552(10) .
Sb1 Br6 2.5570(11) .
Sb1 Br4 2.5598(9) .
C1 N1 1.485(10) .
C1 H1A 0.9800 .
C1 H1B 0.9800 .
C1 H1C 0.9800 .
N1 C6 1.321(12) .
N1 C2 1.328(11) .
C2 C3 1.397(12) .
C2 H2 0.9500 .
C3 C4 1.364(13) .
C3 H3 0.9500 .
C4 C5 1.391(12) .
C4 C7 1.480(12) .
C5 C6 1.383(12) .
C5 H5 0.9500 .
C6 H6 0.9500 .
C7 H7A 0.9800 .
C7 H7B 0.9800 .
C7 H7C 0.9800 .
