#------------------------------------------------------------------------------
#$Date: 2022-03-04 05:16:01 +0200 (Fri, 04 Mar 2022) $
#$Revision: 273320 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/56/65/1566560.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_1566560
loop_
_publ_author_name
'Ghallab, Rochdi'
'Bougueria, Hassiba'
'Merazig, Hocine'
_publ_section_title
;
 4-Amidinopyridinium hexachloridostannate(IV) dihydrate
;
_journal_coeditor_code           HB4399
_journal_issue                   3
_journal_name_full               IUCrData
_journal_page_first              x220195
_journal_paper_doi               10.1107/S241431462200195X
_journal_volume                  7
_journal_year                    2022
_chemical_formula_iupac          '(C6 H9 N3) [Sn Cl6], 2H2 O'
_chemical_formula_moiety         'C6 H9 N3 2+, Cl6 Sn 2-, 2(H2 O)'
_chemical_formula_sum            'C6 H13 Cl6 N3 O2 Sn'
_chemical_formula_weight         490.58
_chemical_name_common
;
4-Amidinopyridinium hexachloridostannate(IV) dihydrate
;
_chemical_name_systematic
;
4-[Amino(iminiumyl)methyl]pyridin-1-ium hexachloridostannate(IV) dihydrate
;
_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   mixed
_atom_sites_solution_primary     iterative
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                105.726(7)
_cell_angle_beta                 97.426(9)
_cell_angle_gamma                112.383(7)
_cell_formula_units_Z            1
_cell_length_a                   7.4224(13)
_cell_length_b                   7.4518(11)
_cell_length_c                   8.4986(16)
_cell_measurement_reflns_used    1889
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      30.5
_cell_measurement_theta_min      5.0
_cell_volume                     403.85(13)
_computing_cell_refinement
;
APEX2 (Bruker, 2016)
;
_computing_data_collection
;
SAINT (Bruker, 2016)
;
_computing_data_reduction
;
SAINT (Bruker, 2016)
;
_computing_molecular_graphics
;
OLEX2 (Dolomanov et al.,  2009)
;
_computing_publication_material
;
OLEX2 (Dolomanov et al.,  2009)
;
_computing_structure_refinement
;
ShelXL (Sheldrick, 2015)
;
_computing_structure_solution
;
olex2.solve (Bourhis et al.,  2015)
;
_diffrn_ambient_temperature      296.15
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'Bruker APEXII CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0276
_diffrn_reflns_av_unetI/netI     0.0420
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            10469
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.507
_diffrn_reflns_theta_min         4.973
_exptl_absorpt_coefficient_mu    2.570
_exptl_absorpt_correction_T_max  0.754
_exptl_absorpt_correction_T_min  0.676
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Bruker, 2016)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.017
_exptl_crystal_description       block
_exptl_crystal_F_000             238
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.11
_refine_diff_density_max         1.215
_refine_diff_density_min         -1.352
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.149
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     154
_refine_ls_number_reflns         2442
_refine_ls_number_restraints     53
_refine_ls_restrained_S_all      1.142
_refine_ls_R_factor_all          0.0753
_refine_ls_R_factor_gt           0.0458
_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)+(0.0167P)²+0.8036P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0779
_refine_ls_wR_factor_ref         0.0852
_reflns_number_gt                1889
_reflns_number_total             2442
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            hb4399sup1.cif
_cod_data_source_block           I
_cod_original_cell_volume        403.85(12)
_cod_database_code               1566560
_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, -y, -z'
loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Sn Sn1 0.000000 0.500000 0.500000 0.04673(15) Uani d 1 . .
Cl Cl2 -0.0563(2) 0.39683(16) 0.19228(11) 0.0675(4) Uani d 1 . .
Cl Cl1B 0.2964(10) 0.7987(8) 0.5355(8) 0.0640(13) Uani d 0.5 A 1
Cl Cl3B 0.2133(9) 0.3209(8) 0.5250(8) 0.0607(14) Uani d 0.33 A 1
Cl Cl1A 0.3472(10) 0.7539(8) 0.5316(7) 0.0612(12) Uani d 0.5 A 2
Cl Cl3A 0.1294(5) 0.2493(4) 0.4986(4) 0.0711(9) Uani d 0.67 A 2
C C3 0.470(3) 1.475(3) 0.998(2) 0.039(3) Uani d 0.5 B -1
C C4 0.5060(13) 1.6621(11) 1.1133(9) 0.0462(19) Uani d 0.5 B -1
H H4 0.465642 1.667299 1.212925 0.055 Uiso calc 0.5 B -1
C C5 0.5998(16) 1.8390(14) 1.0820(13) 0.062(2) Uani d 0.5 B -1
H H5 0.618436 1.965008 1.157590 0.074 Uiso calc 0.5 B -1
N N1 0.666(2) 1.8325(16) 0.9421(16) 0.081(3) Uani d 0.5 B -1
H H1 0.734961 1.946420 0.927815 0.097 Uiso calc 0.5 B -1
C C1 0.625(3) 1.6494(18) 0.8222(18) 0.088(5) Uani d 0.5 B -1
H H1A 0.661958 1.646634 0.721374 0.105 Uiso calc 0.5 B -1
C C2 0.5291(16) 1.4684(15) 0.8517(10) 0.059(2) Uani d 0.5 B -1
H H2 0.504299 1.342167 0.772395 0.071 Uiso calc 0.5 B -1
C C6 0.3621(14) 1.2750(14) 1.0199(13) 0.053(2) Uani d 0.5 B -1
N N2 0.227(2) 1.1247(14) 0.8868(15) 0.099(4) Uani d 0.5 B -1
H H2A 0.153059 1.008127 0.895028 0.119 Uiso calc 0.5 B -1
H H2B 0.211066 1.142421 0.790976 0.119 Uiso calc 0.5 B -1
N N3 0.397(2) 1.2666(18) 1.1621(18) 0.089(5) Uani d 0.5 B -1
H H3A 0.329233 1.154902 1.180199 0.106 Uiso calc 0.5 B -1
H H3B 0.488756 1.372373 1.243683 0.106 Uiso calc 0.5 B -1
O O1WA 0.0858(13) 1.8847(11) 1.1795(10) 0.069(2) Uani d 0.5 C 1
H H1WA 0.119362 1.785736 1.167388 0.103 Uiso d 0.5 C 1
H H1WB 0.101422 1.945036 1.284078 0.103 Uiso d 0.5 C 1
O O1WB 0.2372(18) 1.8798(12) 1.1997(9) 0.091(3) Uani d 0.5 D 2
H H1WC 0.297336 1.913349 1.302646 0.137 Uiso d 0.5 D 2
H H1WD 0.110355 1.828348 1.187657 0.137 Uiso d 0.5 D 2
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'
Cl Cl 0.1484 0.1585 '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'
O O 0.0106 0.0060 '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_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
Cl2 Sn1 Cl2 . 2_566 180.0 ?
Cl2 Sn1 Cl3B . 2_566 87.17(16) ?
Cl2 Sn1 Cl3B 2_566 2_566 92.83(16) ?
Cl2 Sn1 Cl3B . . 92.83(16) ?
Cl2 Sn1 Cl3B 2_566 . 87.17(16) ?
Cl2 Sn1 Cl1A 2_566 . 90.98(14) ?
Cl2 Sn1 Cl1A . . 89.02(14) ?
Cl2 Sn1 Cl1A . 2_566 90.98(14) ?
Cl2 Sn1 Cl1A 2_566 2_566 89.02(14) ?
Cl1B Sn1 Cl2 . 2_566 89.79(15) ?
Cl1B Sn1 Cl2 . . 90.21(15) ?
Cl1B Sn1 Cl2 2_566 . 89.79(15) ?
Cl1B Sn1 Cl2 2_566 2_566 90.21(15) ?
Cl1B Sn1 Cl1B 2_566 . 180.0 ?
Cl1B Sn1 Cl3B . . 87.92(17) ?
Cl1B Sn1 Cl3B 2_566 . 92.08(17) ?
Cl1B Sn1 Cl3B 2_566 2_566 87.92(17) ?
Cl1B Sn1 Cl3B . 2_566 92.08(17) ?
Cl1B Sn1 Cl1A . 2_566 166.23(14) ?
Cl1B Sn1 Cl1A 2_566 2_566 13.77(14) ?
Cl1B Sn1 Cl3A 2_566 2_566 101.89(14) ?
Cl1B Sn1 Cl3A . 2_566 78.11(14) ?
Cl3B Sn1 Cl3B . 2_566 180.0 ?
Cl3B Sn1 Cl1A . 2_566 105.72(16) ?
Cl3B Sn1 Cl1A 2_566 2_566 74.28(16) ?
Cl3A Sn1 Cl2 . . 89.55(8) ?
Cl3A Sn1 Cl2 2_566 . 90.45(8) ?
Cl3A Sn1 Cl1A . . 88.16(12) ?
Cl3A Sn1 Cl1A 2_566 . 91.84(12) ?
Cl3A Sn1 Cl3A 2_566 . 180.0 ?
C4 C3 C6 . . 123.3(12) ?
C2 C3 C4 . . 119.7(15) ?
C2 C3 C6 . . 117.0(12) ?
C5 C4 C3 . . 120.1(10) ?
N1 C5 C4 . . 120.0(9) ?
C5 N1 C1 . . 121.3(9) ?
N1 C1 C2 . . 119.2(10) ?
C3 C2 C1 . . 119.5(11) ?
N2 C6 C3 . . 116.5(11) ?
N3 C6 C3 . . 118.0(11) ?
N3 C6 N2 . . 125.4(11) ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Sn1 Cl2 . 2.4470(10) ?
Sn1 Cl2 2_566 2.4470(10) ?
Sn1 Cl1B 2_566 2.371(6) ?
Sn1 Cl1B . 2.371(6) ?
Sn1 Cl3B 2_566 2.451(7) ?
Sn1 Cl3B . 2.451(7) ?
Sn1 Cl1A . 2.475(7) ?
Sn1 Cl1A 2_566 2.475(7) ?
Sn1 Cl3A 2_566 2.402(4) ?
Sn1 Cl3A . 2.402(4) ?
C3 C4 . 1.372(15) ?
C3 C2 . 1.366(15) ?
C3 C6 . 1.48(2) ?
C4 C5 . 1.354(10) ?
C5 N1 . 1.339(11) ?
N1 C1 . 1.358(12) ?
C1 C2 . 1.374(12) ?
C6 N2 . 1.306(14) ?
C6 N3 . 1.226(16) ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_publ_flag
N1 H1 O1WA 2_697 0.86 1.96 2.760(15) 154 yes
N1 H1 O1WB 2_697 0.86 1.87 2.649(15) 149 yes
N2 H2A Cl2 2_566 0.86 2.68 3.431(11) 147 yes
N3 H3A O1WA 1_545 0.86 2.13 2.961(16) 162 yes
N3 H3A O1WB 1_545 0.86 1.96 2.795(16) 163 yes
N3 H3B Cl1A 2_677 0.86 2.69 3.093(16) 110 yes
N3 H3B Cl3B 2_677 0.86 2.56 3.420(16) 175 yes
O1WA H1WA Cl2 1_566 0.85 2.77 3.415(8) 134 yes
O1WA H1WB Cl3A 1_576 0.85 2.41 3.154(9) 147 yes
O1WB H1WC Cl1A 1_566 0.85 2.60 3.305(10) 142 yes
O1WB H1WC Cl1B 1_566 0.85 2.36 3.085(10) 144 yes
O1WB H1WC Cl1A 2_687 0.85 2.69 3.251(12) 124 yes
O1WB H1WC Cl1B 2_687 0.85 2.83 3.396(13) 126 yes
C1 H1A Cl3A 2_676 0.93 2.67 3.561(17) 161 yes
C1 H1A Cl3B 2_676 0.93 2.43 3.356(17) 174 yes
C5 H5 Cl1A 2_687 0.93 2.80 3.674(12) 157 yes
C5 H5 Cl1B 2_687 0.93 2.56 3.385(12) 149 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_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion
_geom_torsion_publ_flag
C5 N1 C1 C2 . . . . -6(3) no
C1 N1 C5 C4 . . . . 6(2) no
N1 C1 C2 C3 . . . . 2(3) no
C1 C2 C3 C4 . . . . 0(3) no
C1 C2 C3 C6 . . . . 178.1(16) no
C6 C3 C4 C5 . . . . -177.7(14) no
C2 C3 C6 N2 . . . . -42(2) no
C2 C3 C6 N3 . . . . 142.5(16) no
C4 C3 C6 N2 . . . . 135.9(17) no
C4 C3 C6 N3 . . . . -40(3) no
C2 C3 C4 C5 . . . . 0(3) no
C3 C4 C5 N1 . . . . -3(2) no

_cod_database_fobs_code 1566560
