#------------------------------------------------------------------------------
#$Date: 2024-08-07 04:59:08 +0300 (Wed, 07 Aug 2024) $
#$Revision: 294020 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/02/32/2023235.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_2023235
loop_
_publ_author_name
'Röwekamp-Krugley, Natalia'
'Reuter, Hans'
_publ_section_title
;
 [SnF(bipy)(H2O)]2[SnF6], a mixed-valent inorganic tin(II)--tin(IV)
 compound
;
_journal_coeditor_code           OI2009
_journal_issue                   9
_journal_name_full
'Acta Crystallographica Section E Crystallographic Communications'
_journal_paper_doi               10.1107/S2056989024007400
_journal_volume                  80
_journal_year                    2024
_chemical_formula_iupac          '[Sn F (C10 H8 N2) (H2 O1)]2 [Sn F6]'
_chemical_formula_moiety         '2(C10 H10 F1 N2 O1 Sn +), F6 Sn 2-'
_chemical_formula_sum            'C20 H20 F8 N4 O2 Sn3'
_chemical_formula_weight         856.47
_chemical_name_systematic
;
Bis[aqua(2,2'-bipyridine)fluoridotin(II)] hexafluoridotin(IV)
;
_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     direct
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                97.073(2)
_cell_angle_beta                 98.474(2)
_cell_angle_gamma                100.644(2)
_cell_formula_units_Z            1
_cell_length_a                   7.4579(4)
_cell_length_b                   8.4601(5)
_cell_length_c                   9.8864(6)
_cell_measurement_reflns_used    9888
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.85
_cell_measurement_theta_min      2.48
_cell_volume                     599.06(6)
_computing_cell_refinement
;
SAINT (Bruker, 2009)
;
_computing_data_collection
;
APEX2 (Bruker, 2009)
;
_computing_data_reduction
;
SAINT (Bruker, 2009)
;
_computing_molecular_graphics
;
DIAMOND (Brandenburg, 2006), Mercury (Macrae et al.
(2020)
;
_computing_publication_material
;
publCIF (Westrip, 2010)
;
_computing_structure_refinement
;
SHELXL2014/7 (Sheldrick, 2015)
;
_computing_structure_solution
;
SHELXS97 (Sheldrick 2008)
;
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.990
_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  0.0626
_diffrn_reflns_av_unetI/netI     0.0336
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            28904
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.996
_diffrn_reflns_theta_min         2.996
_exptl_absorpt_coefficient_mu    3.193
_exptl_absorpt_correction_T_max  0.713
_exptl_absorpt_correction_T_min  0.434
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Krause et al.,  2015
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.374
_exptl_crystal_description       plate
_exptl_crystal_F_000             406
_exptl_crystal_size_max          0.168
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.047
_refine_diff_density_max         0.887
_refine_diff_density_min         -0.693
_refine_ls_extinction_coef       0.0061(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method
;
SHELXL2014/7 (Sheldrick, 2015)
;
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    refU
_refine_ls_matrix_type           full
_refine_ls_number_parameters     172
_refine_ls_number_reflns         2864
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.0262
_refine_ls_R_factor_gt           0.0223
_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)+(0.0240P)²+0.4078P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0517
_refine_ls_wR_factor_ref         0.0533
_reflns_number_gt                2611
_reflns_number_total             2864
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            oi2009.cif
_cod_data_source_block           I
_cod_database_code               2023235
_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   0.616
_shelx_estimated_absorpt_t_max   0.864
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 0.5000 1.0000 1.0000 0.01059(8) Uani d 1 . .
F F11 0.22638(19) 0.91895(18) 0.96683(15) 0.0190(3) Uani d 1 . .
F F12 0.5060(2) 0.96203(18) 0.80238(14) 0.0192(3) Uani d 1 . .
F F13 0.4618(2) 1.21909(17) 0.98795(15) 0.0198(3) Uani d 1 . .
Sn Sn2 0.21949(2) 0.11033(2) 0.42958(2) 0.01159(8) Uani d 1 . .
F F21 -0.05571(18) 0.10252(17) 0.41199(14) 0.0143(3) Uani d 1 . .
N N1 0.2719(3) 0.3727(2) 0.3702(2) 0.0124(4) Uani d 1 . .
C C1 0.3234(3) 0.3987(3) 0.2477(3) 0.0150(5) Uani d 1 . .
H H1 0.3362 0.3083 0.1854 0.015(2) Uiso calc 1 . .
C C2 0.3578(3) 0.5513(3) 0.2103(2) 0.0161(6) Uani d 1 . .
H H2 0.3939 0.5660 0.1237 0.015(2) Uiso calc 1 . .
C C3 0.3388(3) 0.6832(3) 0.3011(3) 0.0169(5) Uani d 1 . .
H H3 0.3597 0.7895 0.2769 0.015(2) Uiso calc 1 . .
C C4 0.2890(3) 0.6585(3) 0.4277(3) 0.0149(5) Uani d 1 . .
H H4 0.2761 0.7477 0.4914 0.015(2) Uiso calc 1 . .
C C5 0.2581(3) 0.5018(3) 0.4601(2) 0.0125(5) Uani d 1 . .
C C6 0.2159(3) 0.4654(3) 0.5971(2) 0.0120(5) Uani d 1 . .
N N2 0.2082(3) 0.3096(2) 0.6171(2) 0.0118(4) Uani d 1 . .
C C7 0.1811(3) 0.2676(3) 0.7394(2) 0.0152(5) Uani d 1 . .
H H7 0.1791 0.1582 0.7534 0.015(2) Uiso calc 1 . .
C C8 0.1557(4) 0.3780(3) 0.8464(3) 0.0174(5) Uani d 1 . .
H H8 0.1343 0.3447 0.9319 0.015(2) Uiso calc 1 . .
C C9 0.1622(3) 0.5373(3) 0.8268(3) 0.0167(5) Uani d 1 . .
H H9 0.1450 0.6151 0.8991 0.015(2) Uiso calc 1 . .
C C10 0.1940(3) 0.5838(3) 0.7003(2) 0.0135(5) Uani d 1 . .
H H10 0.2006 0.6934 0.6852 0.015(2) Uiso calc 1 . .
O O1 0.0938(2) 0.0501(2) 0.18594(17) 0.0187(4) Uani d 1 . .
H H101 -0.0229 0.0670 0.1412 0.073(10) Uiso d 1 . .
H H102 0.1481 0.0034 0.1126 0.073(10) Uiso d 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 0.0000 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'
F F 0.0171 0.0103 '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 0.0060 '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
F13 Sn1 F13 . 2_677 180.0 ?
F13 Sn1 F12 . 2_677 89.28(6) ?
F13 Sn1 F12 2_677 2_677 90.72(6) ?
F13 Sn1 F12 . . 90.72(6) ?
F13 Sn1 F12 2_677 . 89.28(6) ?
F12 Sn1 F12 2_677 . 180.00(9) ?
F13 Sn1 F11 . . 89.59(6) ?
F13 Sn1 F11 2_677 . 90.41(6) ?
F12 Sn1 F11 2_677 . 88.39(6) ?
F12 Sn1 F11 . . 91.61(6) ?
F13 Sn1 F11 . 2_677 90.41(6) ?
F13 Sn1 F11 2_677 2_677 89.59(6) ?
F12 Sn1 F11 2_677 2_677 91.62(6) ?
F12 Sn1 F11 . 2_677 88.39(6) ?
F11 Sn1 F11 . 2_677 180.00(3) ?
F21 Sn2 N1 . . 91.52(6) ?
F21 Sn2 N2 . . 78.11(6) ?
N1 Sn2 N2 . . 68.50(7) ?
F21 Sn2 O1 . . 73.42(6) ?
N1 Sn2 O1 . . 79.62(6) ?
N2 Sn2 O1 . . 136.22(6) ?
C5 N1 C1 . . 118.7(2) ?
C5 N1 Sn2 . . 120.40(15) ?
C1 N1 Sn2 . . 120.81(16) ?
N1 C1 C2 . . 122.4(2) ?
N1 C1 H1 . . 118.8 ?
C2 C1 H1 . . 118.8 ?
C1 C2 C3 . . 118.8(2) ?
C1 C2 H2 . . 120.6 ?
C3 C2 H2 . . 120.6 ?
C4 C3 C2 . . 119.3(2) ?
C4 C3 H3 . . 120.3 ?
C2 C3 H3 . . 120.3 ?
C3 C4 C5 . . 119.1(2) ?
C3 C4 H4 . . 120.4 ?
C5 C4 H4 . . 120.4 ?
N1 C5 C4 . . 121.6(2) ?
N1 C5 C6 . . 115.7(2) ?
C4 C5 C6 . . 122.7(2) ?
N2 C6 C10 . . 121.7(2) ?
N2 C6 C5 . . 115.3(2) ?
C10 C6 C5 . . 122.9(2) ?
C7 N2 C6 . . 119.5(2) ?
C7 N2 Sn2 . . 120.78(16) ?
C6 N2 Sn2 . . 119.55(15) ?
N2 C7 C8 . . 122.1(2) ?
N2 C7 H7 . . 118.9 ?
C8 C7 H7 . . 118.9 ?
C9 C8 C7 . . 118.8(2) ?
C9 C8 H8 . . 120.6 ?
C7 C8 H8 . . 120.6 ?
C8 C9 C10 . . 119.7(2) ?
C8 C9 H9 . . 120.2 ?
C10 C9 H9 . . 120.2 ?
C6 C10 C9 . . 118.1(2) ?
C6 C10 H10 . . 121.0 ?
C9 C10 H10 . . 121.0 ?
Sn2 O1 H101 . . 127.2 ?
Sn2 O1 H102 . . 127.9 ?
H101 O1 H102 . . 105.0 ?
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 F13 . 1.9418(14) ?
Sn1 F13 2_677 1.9418(14) ?
Sn1 F12 2_677 1.9491(14) ?
Sn1 F12 . 1.9491(14) ?
Sn1 F11 . 1.9931(14) ?
Sn1 F11 2_677 1.9931(14) ?
Sn2 F21 . 2.0221(13) ?
Sn2 N1 . 2.344(2) ?
Sn2 N2 . 2.369(2) ?
Sn2 O1 . 2.4076(17) ?
N1 C5 . 1.350(3) ?
N1 C1 . 1.354(3) ?
C1 C2 . 1.375(3) ?
C1 H1 . 0.9500 ?
C2 C3 . 1.386(3) ?
C2 H2 . 0.9500 ?
C3 C4 . 1.385(4) ?
C3 H3 . 0.9500 ?
C4 C5 . 1.389(3) ?
C4 H4 . 0.9500 ?
C5 C6 . 1.490(3) ?
C6 N2 . 1.349(3) ?
C6 C10 . 1.389(3) ?
N2 C7 . 1.335(3) ?
C7 C8 . 1.381(4) ?
C7 H7 . 0.9500 ?
C8 C9 . 1.378(4) ?
C8 H8 . 0.9500 ?
C9 C10 . 1.396(3) ?
C9 H9 . 0.9500 ?
C10 H10 . 0.9500 ?
O1 H101 . 0.9600 ?
O1 H102 . 0.9600 ?
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
O1 H101 F11 2_566 0.96 1.75 2.705(2) 170.0
O1 H102 F11 1_544 0.96 1.75 2.710(2) 174.0
