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#$Date: 2021-11-30 12:26:09 +0200 (Tue, 30 Nov 2021) $
#$Revision: 270940 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/56/54/1565455.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_1565455
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            '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       'ω 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/[σ²(Fo²)+(0.0118P)²] where P=(Fo²+2Fc²)/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 > 2σ(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_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   0.160
_shelx_estimated_absorpt_t_max   0.340
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'
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 0.5000 0.0000 0.5000 0.01357(9) Uani 1 2 d S . P . .
C1 C 0.3145(3) 0.4200(5) 0.2513(2) 0.0226(9) Uani 1 1 d . . . . .
H1A H 0.3250 0.3278 0.2115 0.034 Uiso 1 1 calc R U . . .
H1B H 0.2317 0.4598 0.2417 0.034 Uiso 1 1 calc R U . . .
H1C H 0.3356 0.3683 0.3055 0.034 Uiso 1 1 calc R U . . .
N1 N 0.5190(3) 0.5222(4) 0.25120(18) 0.0166(7) Uani 1 1 d . . . . .
Br1 Br 0.31930(3) 0.21011(5) 0.47437(2) 0.02289(11) Uani 1 1 d . . . . .
Br2 Br 0.51944(3) 0.02779(5) 0.35213(2) 0.01889(10) Uani 1 1 d . . . . .
C2 C 0.3934(3) 0.5804(5) 0.2441(2) 0.0189(9) Uani 1 1 d . . . . .
H2A H 0.3668 0.6403 0.1914 0.023 Uiso 1 1 calc R U . . .
H2B H 0.3871 0.6696 0.2868 0.023 Uiso 1 1 calc R U . . .
Br3 Br 0.63566(4) 0.27424(5) 0.53533(2) 0.02236(10) Uani 1 1 d . . . . .
C3 C 0.5857(3) 0.5146(5) 0.3267(2) 0.0215(9) Uani 1 1 d . . . . .
H3 H 0.5515 0.5468 0.3716 0.026 Uiso 1 1 calc R U . . .
Br4 Br 0.43875(4) 0.00623(5) 0.13671(2) 0.02605(11) Uani 1 1 d . . . . .
C4 C 0.7014(4) 0.4612(5) 0.3381(3) 0.0285(10) Uani 1 1 d . . . . .
H4 H 0.7480 0.4571 0.3908 0.034 Uiso 1 1 calc R U . . .
Br5 Br 0.5000 0.0000 0.0000 0.01940(13) Uani 1 2 d S . P . .
C5 C 0.7501(4) 0.4131(6) 0.2727(3) 0.0313(11) Uani 1 1 d . . . . .
H5 H 0.8307 0.3768 0.2798 0.038 Uiso 1 1 calc R U . . .
C7 C 0.5644(4) 0.4733(5) 0.1862(2) 0.0217(9) Uani 1 1 d . . . . .
C6 C 0.6811(4) 0.4181(5) 0.1969(3) 0.0280(10) Uani 1 1 d . . . . .
H6 H 0.7140 0.3834 0.1517 0.034 Uiso 1 1 calc R U . . .
C8 C 0.4891(4) 0.4849(5) 0.1040(2) 0.0309(11) Uani 1 1 d . . . . .
H8A H 0.4130 0.4249 0.1042 0.046 Uiso 1 1 calc R U . . .
H8B H 0.5295 0.4246 0.0652 0.046 Uiso 1 1 calc R U . . .
H8C H 0.4754 0.6127 0.0890 0.046 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'
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'
H H 0.0000 0.0000 '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
Br3 Sb1 Br3 180.0 . 3_656
Br3 Sb1 Br1 89.861(13) . 3_656
Br3 Sb1 Br1 90.139(13) 3_656 3_656
Br3 Sb1 Br1 90.140(13) . .
Br3 Sb1 Br1 89.860(13) 3_656 .
Br1 Sb1 Br1 180.000(11) 3_656 .
Br3 Sb1 Br2 90.269(12) . .
Br3 Sb1 Br2 89.732(12) 3_656 .
Br1 Sb1 Br2 89.860(13) 3_656 .
Br1 Sb1 Br2 90.140(13) . .
Br3 Sb1 Br2 89.731(12) . 3_656
Br3 Sb1 Br2 90.268(12) 3_656 3_656
Br1 Sb1 Br2 90.141(13) 3_656 3_656
Br1 Sb1 Br2 89.859(13) . 3_656
Br2 Sb1 Br2 180.0 . 3_656
C2 C1 H1A 109.5 . .
C2 C1 H1B 109.5 . .
H1A C1 H1B 109.5 . .
C2 C1 H1C 109.5 . .
H1A C1 H1C 109.5 . .
H1B C1 H1C 109.5 . .
C7 N1 C3 121.1(3) . .
C7 N1 C2 121.8(3) . .
C3 N1 C2 117.1(3) . .
N1 C2 C1 110.9(3) . .
N1 C2 H2A 109.5 . .
C1 C2 H2A 109.5 . .
N1 C2 H2B 109.5 . .
C1 C2 H2B 109.5 . .
H2A C2 H2B 108.0 . .
N1 C3 C4 120.5(4) . .
N1 C3 H3 119.7 . .
C4 C3 H3 119.7 . .
C3 C4 C5 119.4(4) . .
C3 C4 H4 120.3 . .
C5 C4 H4 120.3 . .
Br4 Br5 Br4 180.0 3_655 .
C6 C5 C4 119.5(4) . .
C6 C5 H5 120.2 . .
C4 C5 H5 120.2 . .
N1 C7 C6 119.1(4) . .
N1 C7 C8 119.8(4) . .
C6 C7 C8 121.1(4) . .
C5 C6 C7 120.4(4) . .
C5 C6 H6 119.8 . .
C7 C6 H6 119.8 . .
C7 C8 H8A 109.5 . .
C7 C8 H8B 109.5 . .
H8A C8 H8B 109.5 . .
C7 C8 H8C 109.5 . .
H8A C8 H8C 109.5 . .
H8B C8 H8C 109.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Sb1 Br3 2.5525(4) .
Sb1 Br3 2.5525(4) 3_656
Sb1 Br1 2.5604(4) 3_656
Sb1 Br1 2.5605(4) .
Sb1 Br2 2.5624(4) .
Sb1 Br2 2.5624(4) 3_656
C1 C2 1.507(5) .
C1 H1A 0.9800 .
C1 H1B 0.9800 .
C1 H1C 0.9800 .
N1 C7 1.351(5) .
N1 C3 1.363(4) .
N1 C2 1.488(4) .
C2 H2A 0.9900 .
C2 H2B 0.9900 .
C3 C4 1.365(5) .
C3 H3 0.9500 .
Br4 Br5 2.5420(4) .
C4 C5 1.377(6) .
C4 H4 0.9500 .
Br5 Br4 2.5420(4) 3_655
C5 C6 1.376(5) .
C5 H5 0.9500 .
C7 C6 1.380(5) .
C7 C8 1.498(5) .
C6 H6 0.9500 .
C8 H8A 0.9800 .
C8 H8B 0.9800 .
C8 H8C 0.9800 .
