#------------------------------------------------------------------------------
#$Date: 2022-05-10 11:34:53 +0300 (Tue, 10 May 2022) $
#$Revision: 275299 $
#$URL: file:///home/coder/svn-repositories/cod/cif/8/10/52/8105205.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_8105205
loop_
_publ_author_name
'Reiss, Guido J.'
'van Megen, Martin'
_publ_section_title
;
 The twinned crystal structure of
 [4,4′-bipyridine]-1,1′-diium hexachloridostannate(IV),
 C10H10N2SnCl6
;
_journal_issue                   2
_journal_name_full
'Zeitschrift für Kristallographie - New Crystal Structures'
_journal_page_first              281
_journal_page_last               284
_journal_paper_doi               10.1515/ncrs-2021-0443
_journal_volume                  237
_journal_year                    2022
_chemical_formula_moiety         'C10 H10 N2, Cl6 Sn'
_chemical_formula_sum            'C10 H10 Cl6 N2 Sn'
_chemical_formula_weight         489.59
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-I 2ya'
_space_group_name_H-M_alt        'I 1 2/a 1'
_atom_sites_solution_hydrogens   difmap
_audit_creation_method           SHELXL-2018/3
_cell_angle_alpha                90
_cell_angle_beta                 93.042(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.4941(3)
_cell_length_b                   12.8731(4)
_cell_length_c                   15.8688(5)
_cell_measurement_reflns_used    3749
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.69
_cell_measurement_theta_min      3.15
_cell_volume                     1528.74(9)
_computing_cell_refinement       'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Diamond, Crystal Impact'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       omega
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_unetI/netI     0.0372
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            3193
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        27.597
_diffrn_reflns_theta_max         27.597
_diffrn_reflns_theta_min         4.327
_diffrn_source                   'fine-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    2.705
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.79296
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.93a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.127
_exptl_crystal_description       block
_exptl_crystal_F_000             944
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.147
_exptl_crystal_size_min          0.118
_refine_diff_density_max         1.434
_refine_diff_density_min         -0.476
_refine_diff_density_rms         0.124
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    refxyz
_refine_ls_matrix_type           full
_refine_ls_number_parameters     105
_refine_ls_number_reflns         3193
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.0434
_refine_ls_R_factor_gt           0.0264
_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)+(0.0176P)²+0.2300P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0467
_refine_ls_wR_factor_ref         0.0485
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2334
_reflns_number_total             3193
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            suppl_j_ncrs-2021-0443_suppl.cif
_cod_data_source_block           exp_623_100_twin1_hklf5
_cod_original_cell_volume        1528.73(9)
_cod_original_sg_symbol_H-M      'I 2/a'
_cod_database_code               8105205
_shelx_shelxl_version_number     2018/3
_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.
;
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y, -z'
'x+1/2, y+1/2, z+1/2'
'-x+1, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y, z'
'-x+1/2, -y+1/2, -z+1/2'
'x, -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
Sn1 Sn 0.250000 0.250000 0.250000 0.01118(8) Uani 1 2 d S . P . .
Cl1 Cl 0.29832(11) 0.26028(6) 0.40446(4) 0.01923(18) Uani 1 1 d . . . . .
Cl2 Cl 0.10352(11) 0.41644(5) 0.25078(4) 0.01688(17) Uani 1 1 d . . . . .
Cl3 Cl -0.03375(11) 0.16763(6) 0.26519(5) 0.02192(18) Uani 1 1 d . . . . .
N1 N 0.750000 0.5090(3) 0.500000 0.0208(9) Uani 1 2 d DS T P . .
H1N H 0.750000 0.5728(19) 0.500000 0.025 Uiso 1 2 d DS U P . .
N2 N 0.750000 -0.0305(3) 0.500000 0.0186(9) Uani 1 2 d DS T P . .
H2N H 0.750000 -0.0962(19) 0.500000 0.022 Uiso 1 2 d DS U P . .
C1 C 0.8004(5) 0.4588(3) 0.4309(2) 0.0196(7) Uani 1 1 d . . . . .
H1 H 0.840(5) 0.499(3) 0.388(2) 0.024 Uiso 1 1 d . U . . .
C2 C 0.8016(5) 0.3523(2) 0.42975(19) 0.0159(7) Uani 1 1 d . . . . .
H2 H 0.839(5) 0.317(2) 0.383(2) 0.019 Uiso 1 1 d . U . . .
C3 C 0.750000 0.2966(3) 0.500000 0.0130(10) Uani 1 2 d S T P . .
C4 C 0.750000 0.1815(3) 0.500000 0.0131(9) Uani 1 2 d S T P . .
C5 C 0.6980(5) 0.1257(2) 0.42720(19) 0.0154(7) Uani 1 1 d . . . . .
H5 H 0.656(5) 0.157(2) 0.378(2) 0.018 Uiso 1 1 d . U . . .
C6 C 0.6982(5) 0.0197(3) 0.4286(2) 0.0183(7) Uani 1 1 d . . . . .
H6 H 0.663(5) -0.015(3) 0.386(2) 0.022 Uiso 1 1 d . 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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Sn Sn -0.6537 1.4246 '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
Cl3 Sn1 Cl3 180.0 7 .
Cl3 Sn1 Cl2 89.20(3) 7 7
Cl3 Sn1 Cl2 90.80(3) . 7
Cl3 Sn1 Cl2 90.80(3) 7 .
Cl3 Sn1 Cl2 89.20(3) . .
Cl2 Sn1 Cl2 180.0 7 .
Cl3 Sn1 Cl1 90.46(3) 7 7
Cl3 Sn1 Cl1 89.54(3) . 7
Cl2 Sn1 Cl1 89.43(2) 7 7
Cl2 Sn1 Cl1 90.57(2) . 7
Cl3 Sn1 Cl1 89.54(3) 7 .
Cl3 Sn1 Cl1 90.46(3) . .
Cl2 Sn1 Cl1 90.57(2) 7 .
Cl2 Sn1 Cl1 89.43(2) . .
Cl1 Sn1 Cl1 180.0 7 .
C1 N1 C1 122.6(4) 2_656 .
C1 N1 H1N 118.7(2) 2_656 .
C1 N1 H1N 118.7(2) . .
C6 N2 C6 122.5(4) 2_656 .
C6 N2 H2N 118.7(2) 2_656 .
C6 N2 H2N 118.7(2) . .
N1 C1 C2 119.6(3) . .
N1 C1 H1 117(2) . .
C2 C1 H1 123(2) . .
C1 C2 C3 120.0(3) . .
C1 C2 H2 120.0(19) . .
C3 C2 H2 120(2) . .
C2 C3 C2 118.2(4) 2_656 .
C2 C3 C4 120.9(2) 2_656 .
C2 C3 C4 120.9(2) . .
C5 C4 C5 118.2(4) . 2_656
C5 C4 C3 120.9(2) . .
C5 C4 C3 120.9(2) 2_656 .
C6 C5 C4 120.0(3) . .
C6 C5 H5 117(2) . .
C4 C5 H5 123(2) . .
N2 C6 C5 119.6(3) . .
N2 C6 H6 119(2) . .
C5 C6 H6 121(2) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Sn1 Cl3 2.3997(8) 7
Sn1 Cl3 2.3997(8) .
Sn1 Cl2 2.4078(7) 7
Sn1 Cl2 2.4078(7) .
Sn1 Cl1 2.4621(6) 7
Sn1 Cl1 2.4621(6) .
N1 C1 1.344(4) 2_656
N1 C1 1.344(4) .
N1 H1N 0.82(2) .
N2 C6 1.343(4) 2_656
N2 C6 1.343(4) .
N2 H2N 0.85(2) .
C1 C2 1.371(4) .
C1 H1 0.92(3) .
C2 C3 1.398(4) .
C2 H2 0.93(3) .
C3 C4 1.481(6) .
C4 C5 1.398(4) .
C4 C5 1.398(4) 2_656
C5 C6 1.366(4) .
C5 H5 0.91(3) .
C6 H6 0.84(3) .
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
N1 H1N Cl1 0.82(2) 2.67(2) 3.363(4) 143.7(3) 5_666 yes
N1 H1N Cl1 0.82(2) 2.67(2) 3.363(4) 143.7(3) 6_665 yes
N2 H2N Cl1 0.85(2) 2.64(2) 3.352(3) 143.2(3) 5_656 yes
N2 H2N Cl1 0.85(2) 2.64(2) 3.352(3) 143.2(3) 6_655 yes
C1 H1 Cl2 0.92(3) 2.94(3) 3.533(3) 124(3) 6_665 yes
C2 H2 Cl3 0.93(3) 2.88(3) 3.786(3) 166(3) 1_655 yes
C5 H5 Cl2 0.91(3) 2.91(3) 3.564(3) 130(2) 7 yes
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
C1 N1 C1 C2 -0.1(2) 2_656 . . .
N1 C1 C2 C3 0.2(5) . . . .
C1 C2 C3 C2 -0.1(2) . . . 2_656
C1 C2 C3 C4 179.9(2) . . . .
C2 C3 C4 C5 142.3(2) 2_656 . . .
C2 C3 C4 C5 -37.7(2) . . . .
C2 C3 C4 C5 -37.7(2) 2_656 . . 2_656
C2 C3 C4 C5 142.3(2) . . . 2_656
C5 C4 C5 C6 0.3(2) 2_656 . . .
C3 C4 C5 C6 -179.7(2) . . . .
C6 N2 C6 C5 0.3(2) 2_656 . . .
C4 C5 C6 N2 -0.6(5) . . . .
