#------------------------------------------------------------------------------
#$Date: 2018-01-30 09:12:21 +0200 (Tue, 30 Jan 2018) $
#$Revision: 205873 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/24/23/2242351.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_2242351
loop_
_publ_author_name
'Bouchene, Rafika'
'Lecheheb, Zohir'
'Belhouas, Ratiba'
'Bouacida, Sofiane'
_publ_section_title
;
 Synthesis, X-ray diffraction and Hirshfeld surface analysis of two new
 hybrid dihydrate compounds: (C₆H₂₂N₄)[SnCl₆]Cl₂·2H₂O
 and (C₈H₂₄N₄)[SnCl₆]Cl₂·2H₂O
;
_journal_coeditor_code           TX2003
_journal_issue                   2
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              206
_journal_page_last               211
_journal_paper_doi               10.1107/S2056989018001044
_journal_volume                  74
_journal_year                    2018
_chemical_formula_iupac          '(C8 H24 N4) [Sn Cl6] Cl2, 2H2 O'
_chemical_formula_moiety         'C8 H24 N4, Cl6 Sn 2+, 2(Cl -), 2(H2 O)'
_chemical_formula_sum            'C8 H28 Cl8 N4 O2 Sn'
_chemical_formula_weight         614.65
_chemical_name_systematic
;
1,4-Bis(2-ammonioethyl)piperazin-1,4-diium hexachloridostannate(IV)
dichloride dihydrate
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.3
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                93.614(2)
_cell_angle_beta                 101.3570(10)
_cell_angle_gamma                117.021(2)
_cell_formula_units_Z            1
_cell_length_a                   7.0856(2)
_cell_length_b                   7.3269(2)
_cell_length_c                   12.1624(4)
_cell_measurement_reflns_used    5436
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      27.485
_cell_measurement_theta_min      2.91
_cell_volume                     543.01(3)
_computing_cell_refinement
;
SCALEPACK (Otwinowski & Minor, 1997)
;
_computing_data_collection
;
COLLECT (Nonius, 199)
;
_computing_data_reduction
;
DENZO and SCALEPACK (Otwinowski & Minor, 1997)
;
_computing_molecular_graphics
;
ORTEP-3 for Windows (Farrugia, 2012) and DIAMOND (Brandenburg & Berndt,
2001)
;
_computing_publication_material
;
WinGX (Farrugia, 2012)
;
_computing_structure_refinement
;
SHELXL97 (Sheldrick, 2008)
;
_computing_structure_solution
;
SHELXS97 (Sheldrick, 2008)
;
_diffrn_ambient_temperature      295(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device       '95mm CCD camera on κ-goniostat'
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       'CCD rotation images, thick slices'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0143
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            4329
_diffrn_reflns_theta_full        27.51
_diffrn_reflns_theta_max         27.51
_diffrn_reflns_theta_min         3.17
_exptl_absorpt_coefficient_mu    2.171
_exptl_absorpt_correction_T_max  0.893
_exptl_absorpt_correction_T_min  0.745
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Krause et al., 2015)
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.88
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       cube
_exptl_crystal_F_000             306
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.609
_refine_diff_density_min         -0.649
_refine_ls_extinction_coef       0.033(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.132
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     117
_refine_ls_number_reflns         2494
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.132
_refine_ls_R_factor_all          0.0278
_refine_ls_R_factor_gt           0.0251
_refine_ls_shift/su_max          0
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0250P)²+0.3256P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0623
_refine_ls_wR_factor_ref         0.0641
_reflns_number_gt                2319
_reflns_number_total             2494
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            tx2003sup1.cif
_cod_data_source_block           II
_cod_database_code               2242351
loop_
_symmetry_equiv_pos_as_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_refinement_flags
_atom_site_occupancy
_atom_site_symmetry_multiplicity
Sn Sn1 0.5 0.5 0 0.02689(10) Uani d S 1 2
Cl Cl3 0.78922(11) 0.66433(10) 0.17479(5) 0.04033(16) Uani d . 1 1
Cl Cl4 0.17862(10) 0.75981(9) 0.44661(6) 0.03755(16) Uani d . 1 1
Cl Cl1 0.30602(10) 0.66732(10) 0.06748(5) 0.03706(15) Uani d . 1 1
Cl Cl2 0.31206(12) 0.19729(9) 0.08532(6) 0.04023(16) Uani d . 1 1
N N4 0.2782(3) 0.3944(3) 0.42328(16) 0.0239(4) Uani d . 1 1
H H4 0.238(5) 0.484(5) 0.440(2) 0.036 Uiso d . 1 1
C C3 0.0936(4) 0.2192(3) 0.33497(19) 0.0269(5) Uani d . 1 1
H H3A -0.0176 0.1302 0.3709 0.032 Uiso calc R 1 1
H H3B 0.1481 0.1361 0.3005 0.032 Uiso calc R 1 1
O O1W 0.5368(4) 1.0237(5) 0.3102(2) 0.0736(8) Uani d D 1 1
H H1W 0.579(9) 1.068(8) 0.3794(19) 0.11 Uiso d D 1 1
H H2W 0.404(4) 0.939(7) 0.297(5) 0.11 Uiso d D 1 1
N N1 -0.1969(4) 0.1317(3) 0.16070(19) 0.0392(5) Uani d . 1 1
H H1A -0.1568 0.0426 0.1338 0.059 Uiso calc R 1 1
H H1B -0.2451 0.1822 0.1035 0.059 Uiso calc R 1 1
H H1C -0.3032 0.0662 0.195 0.059 Uiso calc R 1 1
C C6 0.6631(4) 0.6818(3) 0.4703(2) 0.0275(5) Uani d . 1 1
H H6A 0.7909 0.7482 0.4404 0.033 Uiso calc R 1 1
H H6B 0.6187 0.7849 0.4884 0.033 Uiso calc R 1 1
C C2 -0.0067(4) 0.3044(4) 0.2435(2) 0.0314(5) Uani d . 1 1
H H2A -0.0531 0.3943 0.2786 0.038 Uiso calc R 1 1
H H2B 0.1021 0.3864 0.2044 0.038 Uiso calc R 1 1
C C5 0.4795(4) 0.5058(4) 0.3805(2) 0.0284(5) Uani d . 1 1
H H5A 0.4439 0.561 0.3136 0.034 Uiso calc R 1 1
H H5B 0.5277 0.4078 0.3582 0.034 Uiso calc R 1 1
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 0 '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'
O O 0.0106 0.006 '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
Cl3 Sn1 Cl3 . 2_665 180
Cl3 Sn1 Cl1 . 2_665 90.31(2)
Cl3 Sn1 Cl1 2_665 2_665 89.69(2)
Cl3 Sn1 Cl1 . . 89.69(2)
Cl3 Sn1 Cl1 2_665 . 90.31(2)
Cl1 Sn1 Cl1 2_665 . 180.00(3)
Cl3 Sn1 Cl2 . . 90.42(2)
Cl3 Sn1 Cl2 2_665 . 89.58(2)
Cl1 Sn1 Cl2 2_665 . 88.55(2)
Cl1 Sn1 Cl2 . . 91.45(2)
Cl3 Sn1 Cl2 . 2_665 89.58(2)
Cl3 Sn1 Cl2 2_665 2_665 90.42(2)
Cl1 Sn1 Cl2 2_665 2_665 91.45(2)
Cl1 Sn1 Cl2 . 2_665 88.55(2)
Cl2 Sn1 Cl2 . 2_665 180
C6 N4 C5 2_666 . 109.02(17)
C6 N4 C3 2_666 . 111.27(17)
C5 N4 C3 . . 112.28(18)
C6 N4 H4 2_666 . 109(2)
C5 N4 H4 . . 107(2)
C3 N4 H4 . . 109(2)
N4 C3 C2 . . 110.33(18)
N4 C3 H3A . . 109.6
C2 C3 H3A . . 109.6
N4 C3 H3B . . 109.6
C2 C3 H3B . . 109.6
H3A C3 H3B . . 108.1
H1W O1W H2W . . 106(5)
C2 N1 H1A . . 109.5
C2 N1 H1B . . 109.5
H1A N1 H1B . . 109.5
C2 N1 H1C . . 109.5
H1A N1 H1C . . 109.5
H1B N1 H1C . . 109.5
N4 C6 C5 2_666 . 111.57(18)
N4 C6 H6A 2_666 . 109.3
C5 C6 H6A . . 109.3
N4 C6 H6B 2_666 . 109.3
C5 C6 H6B . . 109.3
H6A C6 H6B . . 108
N1 C2 C3 . . 110.21(19)
N1 C2 H2A . . 109.6
C3 C2 H2A . . 109.6
N1 C2 H2B . . 109.6
C3 C2 H2B . . 109.6
H2A C2 H2B . . 108.1
N4 C5 C6 . . 111.52(19)
N4 C5 H5A . . 109.3
C6 C5 H5A . . 109.3
N4 C5 H5B . . 109.3
C6 C5 H5B . . 109.3
H5A C5 H5B . . 108
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
Sn1 Cl3 . 2.4265(6)
Sn1 Cl3 2_665 2.4265(6)
Sn1 Cl1 2_665 2.4319(6)
Sn1 Cl1 . 2.4319(6)
Sn1 Cl2 . 2.4331(6)
Sn1 Cl2 2_665 2.4331(6)
N4 C6 2_666 1.500(3)
N4 C5 . 1.503(3)
N4 C3 . 1.503(3)
N4 H4 . 0.85(3)
C3 C2 . 1.520(3)
C3 H3A . 0.97
C3 H3B . 0.97
O1W H1W . 0.826(19)
O1W H2W . 0.836(19)
N1 C2 . 1.479(3)
N1 H1A . 0.89
N1 H1B . 0.89
N1 H1C . 0.89
C6 N4 2_666 1.500(3)
C6 C5 . 1.512(3)
C6 H6A . 0.97
C6 H6B . 0.97
C2 H2A . 0.97
C2 H2B . 0.97
C5 H5A . 0.97
C5 H5B . 0.97
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 H1A Cl3 1_445 0.8900 2.7100 3.397(2) 134.00 yes
N1 H1A Cl2 2_555 0.8900 2.8100 3.431(2) 128.00 yes
N1 H1B Cl1 2_565 0.8900 2.4700 3.343(2) 167.00 yes
N1 H1C O1W 1_445 0.8900 1.9200 2.769(4) 158.00 yes
O1W H1W Cl4 2_676 0.83(2) 2.30(3) 3.079(3) 158(6) yes
O1W H2W Cl4 . 0.83(4) 2.67(5) 3.246(3) 128(5) yes
N4 H4 Cl4 . 0.85(4) 2.24(4) 3.073(2) 164(3) yes
C2 H2B Cl1 . 0.9700 2.7900 3.715(3) 160.00 yes
C6 H6A Cl4 1_655 0.9700 2.7000 3.506(3) 141.00 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
C6 N4 C3 C2 2_666 163.67(19)
C5 N4 C3 C2 . -73.8(2)
N4 C3 C2 N1 . -176.51(19)
C6 N4 C5 C6 2_666 -56.4(3)
C3 N4 C5 C6 . 179.86(18)
N4 C6 C5 N4 2_666 57.8(3)
