#------------------------------------------------------------------------------
#$Date: 2019-06-26 07:19:52 +0300 (Wed, 26 Jun 2019) $
#$Revision: 216560 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/24/29/2242994.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_2242994
loop_
_publ_author_name
'Merkelbach, Johannes'
'Frank, Walter'
_publ_section_title
;
 Synthesis, detailed geometric analysis and bond-valence method evaluation
 of the strength of π-arene bonding of two isotypic cationic prehnitene
 tin(II) complexes:
 [{1,2,3,4-(CH₃)₄C₆H₂}₂Sn₂Cl₂][MCl₄]₂ (M =
 Al and Ga)
;
_journal_coeditor_code           WM5510
_journal_issue                   7
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              1051
_journal_page_last               1056
_journal_paper_doi               10.1107/S2056989019008508
_journal_volume                  75
_journal_year                    2019
_chemical_formula_iupac          '[Ga2 Sn2 Cl10 (C10 H14)2]'
_chemical_formula_moiety         '2(C10 H14), Sn2 Cl2 2+, 2(Ga Cl4 -)'
_chemical_formula_sum            'C20 H28 Cl10 Ga2 Sn2'
_chemical_formula_weight         999.78
_chemical_name_systematic
catena-Poly[[chloridogallate(III)]-tri-μ-chlorido-4':1κ²Cl,1:2κ⁴Cl-[(η⁶-1,2,3,4-tetramethylbenzene)tin(II)]-di-μ-chlorido-2:3κ⁴Cl-[(η⁶-1,2,3,4-tetramethylbenzene)tin(II)]-di-μ-chlorido-3:4κ⁴Cl-[chloridogallate(III)]-μ-chlorido-4:1'κ²Cl]
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_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
_audit_creation_method           SHELXL-2018/3
_cell_angle_alpha                85.424(3)
_cell_angle_beta                 72.805(3)
_cell_angle_gamma                86.886(4)
_cell_formula_units_Z            1
_cell_length_a                   8.7572(4)
_cell_length_b                   9.1310(4)
_cell_length_c                   11.2966(5)
_cell_measurement_reflns_used    21911
_cell_measurement_temperature    213(2)
_cell_measurement_theta_max      59.31
_cell_measurement_theta_min      4.48
_cell_volume                     859.73(7)
_computing_cell_refinement
;
X-Area (Stoe & Cie, 2009)
;
_computing_data_collection
;
X-Area (Stoe & Cie, 2009)
;
_computing_data_reduction
;
X-Area (Stoe & Cie, 2009)
;
_computing_molecular_graphics
;
DIAMOND (Brandenburg, 2018)
;
_computing_publication_material
;
publCIF (Westrip, 2010)
;
_computing_structure_refinement
;
SHELXL-2018/3 (Sheldrick, 2015b)
;
_computing_structure_solution
;
SHELXT 2014/5 (Sheldrick, 2015a)
;
_diffrn_ambient_temperature      213(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Stoe IPDS 2'
_diffrn_measurement_method       ω
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0483
_diffrn_reflns_av_unetI/netI     0.0296
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            17522
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.165
_diffrn_reflns_theta_min         2.239
_exptl_absorpt_coefficient_mu    3.774
_exptl_absorpt_correction_T_max  0.65574
_exptl_absorpt_correction_T_min  0.37624
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(Blessing, 1995)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.931
_exptl_crystal_description       needle
_exptl_crystal_F_000             480
_exptl_crystal_size_max          0.610
_exptl_crystal_size_mid          0.130
_exptl_crystal_size_min          0.030
_refine_diff_density_max         0.712
_refine_diff_density_min         -0.502
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.224
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     158
_refine_ls_number_reflns         4638
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.224
_refine_ls_R_factor_all          0.0393
_refine_ls_R_factor_gt           0.0333
_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)+(0.0176P)²+0.9105P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0666
_refine_ls_wR_factor_ref         0.0685
_reflns_number_gt                4242
_reflns_number_total             4638
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            wm5510sup1.cif
_cod_data_source_block           II
_cod_database_code               2242994
_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   0.207
_shelx_estimated_absorpt_t_max   0.895
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
Sn Sn1 0.52200(3) 0.16597(2) 0.60194(2) 0.02838(6) Uani d 1
Ga Ga1 0.78103(4) 0.41311(3) 0.32615(3) 0.03202(8) Uani d 1
Cl Cl1 0.29875(9) 0.01494(8) 0.55911(7) 0.03389(15) Uani d 1
Cl Cl2 0.52418(10) 0.36331(9) 0.37434(8) 0.03987(17) Uani d 1
Cl Cl3 0.86231(14) 0.32600(11) 0.48157(11) 0.0565(3) Uani d 1
Cl Cl4 0.80145(11) 0.65004(8) 0.30948(10) 0.0477(2) Uani d 1
Cl Cl5 0.90567(15) 0.31991(13) 0.15424(11) 0.0646(3) Uani d 1
C C1 0.6226(4) -0.0506(4) 0.7670(3) 0.0372(7) Uani d 1
H H1 0.670505 -0.133397 0.724495 0.045 Uiso calc 1
C C2 0.4589(4) -0.0435(3) 0.8188(3) 0.0332(6) Uani d 1
H H2 0.397444 -0.121308 0.810744 0.040 Uiso calc 1
C C3 0.3829(4) 0.0773(3) 0.8831(3) 0.0301(6) Uani d 1
C C4 0.4772(4) 0.1935(4) 0.8922(3) 0.0331(6) Uani d 1
C C5 0.6443(4) 0.1853(4) 0.8391(3) 0.0345(6) Uani d 1
C C6 0.7182(4) 0.0618(4) 0.7763(3) 0.0358(7) Uani d 1
C C7 0.2046(4) 0.0785(4) 0.9400(3) 0.0431(8) Uani d 1
H H71 0.156274 0.160251 0.902162 0.065 Uiso calc 1
H H72 0.179189 0.089092 1.028578 0.065 Uiso calc 1
H H73 0.163275 -0.012949 0.926109 0.065 Uiso calc 1
C C8 0.3983(5) 0.3255(4) 0.9602(4) 0.0503(9) Uani d 1
H H81 0.426066 0.413765 0.905725 0.075 Uiso calc 1
H H82 0.434745 0.332000 1.032732 0.075 Uiso calc 1
H H83 0.283145 0.315915 0.986078 0.075 Uiso calc 1
C C9 0.7449(5) 0.3105(5) 0.8505(4) 0.0570(11) Uani d 1
H H91 0.857192 0.285182 0.814368 0.085 Uiso calc 1
H H92 0.725155 0.327596 0.937538 0.085 Uiso calc 1
H H93 0.716585 0.398926 0.807067 0.085 Uiso calc 1
C C10 0.8972(4) 0.0473(5) 0.7176(4) 0.0492(9) Uani d 1
H H101 0.923751 -0.046929 0.681388 0.074 Uiso calc 1
H H102 0.951087 0.053946 0.780598 0.074 Uiso calc 1
H H103 0.931353 0.125718 0.653377 0.074 Uiso calc 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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ga Ga 0.2307 1.6083 '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
Cl1 Sn1 Cl1 . 2_656 79.76(2)
Cl1 Sn1 Cl2 . . 88.37(3)
Cl1 Sn1 Cl2 2_656 . 84.56(3)
Cl1 Sn1 Cl4 . 2_666 73.00(2)
Cl1 Sn1 Cl4 2_656 2_666 147.47(3)
Cl1 Sn1 Cl3 . . 146.02(3)
Cl1 Sn1 Cl3 2_656 . 74.35(3)
Cl2 Sn1 Cl3 . . 67.82(2)
Cl2 Sn1 Cl4 . 2_666 77.33(2)
Cl4 Sn1 Cl3 2_666 . 121.37(3)
Cl1 Sn1 C1 . . 98.21(7)
Cl1 Sn1 C1 2_656 . 79.15(7)
Cl1 Sn1 C2 . . 80.68(7)
Cl1 Sn1 C2 2_656 . 96.61(7)
Cl1 Sn1 C3 . . 88.88(6)
Cl1 Sn1 C3 2_656 . 123.05(6)
Cl1 Sn1 C4 . . 113.52(6)
Cl1 Sn1 C4 2_656 . 131.84(6)
Cl1 Sn1 C5 . . 133.20(6)
Cl1 Sn1 C5 2_656 . 112.86(6)
Cl1 Sn1 C6 . . 125.01(7)
Cl1 Sn1 C6 2_656 . 87.73(7)
Cl2 Sn1 C1 . . 161.00(7)
Cl2 Sn1 C2 . . 168.57(7)
Cl2 Sn1 C3 . . 151.20(6)
Cl2 Sn1 C4 . . 138.75(6)
Cl2 Sn1 C5 . . 135.87(6)
Cl2 Sn1 C6 . . 143.69(7)
C1 Sn1 Cl3 . . 98.11(7)
C2 Sn1 Cl3 . . 123.48(7)
C3 Sn1 Cl3 . . 123.69(6)
C4 Sn1 Cl3 . . 100.17(6)
C5 Sn1 Cl3 . . 78.09(6)
C6 Sn1 Cl3 . . 75.93(7)
C1 Sn1 Cl4 . 2_666 121.62(7)
C2 Sn1 Cl4 . 2_666 96.19(7)
C3 Sn1 Cl4 . 2_666 74.45(6)
Cl4 Sn1 C4 2_666 . 76.64(6)
Cl4 Sn1 C5 2_666 . 98.82(7)
C6 Sn1 Cl4 . 2_666 122.46(6)
Sn1 C1 H1 . . 110.6
Sn1 C2 H2 . . 111.6
Sn1 C3 C7 . . 119.1(2)
Sn1 C4 C8 . . 123.0(2)
Sn1 C5 C9 . . 121.9(2)
Sn1 C6 C10 . . 116.1(2)
Cl5 Ga1 Cl3 . . 113.84(5)
Cl5 Ga1 Cl4 . . 110.73(5)
Cl3 Ga1 Cl4 . . 108.39(4)
Cl5 Ga1 Cl2 . . 109.01(4)
Cl3 Ga1 Cl2 . . 106.43(4)
Cl4 Ga1 Cl2 . . 108.21(4)
Sn1 Cl1 Sn1 . 2_656 100.24(2)
Ga1 Cl2 Sn1 . . 95.14(3)
Ga1 Cl3 Sn1 . . 89.58(3)
Ga1 Cl4 Sn1 . 2_666 115.87(3)
C2 C1 C6 . . 121.5(3)
C2 C1 H1 . . 119.2
C6 C1 H1 . . 119.2
C1 C2 C3 . . 121.1(3)
C1 C2 H2 . . 119.5
C3 C2 H2 . . 119.5
C2 C3 C4 . . 118.4(3)
C2 C3 C7 . . 119.1(3)
C4 C3 C7 . . 122.5(3)
C3 C4 C5 . . 120.1(3)
C3 C4 C8 . . 119.5(3)
C5 C4 C8 . . 120.4(3)
C6 C5 C4 . . 120.4(3)
C6 C5 C9 . . 119.9(3)
C4 C5 C9 . . 119.7(3)
C1 C6 C5 . . 118.4(3)
C1 C6 C10 . . 119.0(3)
C5 C6 C10 . . 122.6(3)
C3 C7 H71 . . 109.5
C3 C7 H72 . . 109.5
H71 C7 H72 . . 109.5
C3 C7 H73 . . 109.5
H71 C7 H73 . . 109.5
H72 C7 H73 . . 109.5
C4 C8 H81 . . 109.5
C4 C8 H82 . . 109.5
H81 C8 H82 . . 109.5
C4 C8 H83 . . 109.5
H81 C8 H83 . . 109.5
H82 C8 H83 . . 109.5
C5 C9 H91 . . 109.5
C5 C9 H92 . . 109.5
H91 C9 H92 . . 109.5
C5 C9 H93 . . 109.5
H91 C9 H93 . . 109.5
H92 C9 H93 . . 109.5
C6 C10 H101 . . 109.5
C6 C10 H102 . . 109.5
H101 C10 H102 . . 109.5
C6 C10 H103 . . 109.5
H101 C10 H103 . . 109.5
H102 C10 H103 . . 109.5
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
Sn1 Cl1 . 2.6299(8)
Sn1 Cl1 2_656 2.6481(7)
Sn1 Cl2 . 3.0155(9)
Sn1 Cl3 . 3.2597(11)
Sn1 Cl4 2_666 3.1499(9)
Sn1 C1 . 2.891(3)
Sn1 C2 . 2.921(3)
Sn1 C3 . 3.104(3)
Sn1 C4 . 3.214(3)
Sn1 C5 . 3.185(3)
Sn1 C6 . 3.043(3)
Sn1 Ga1 . 3.8987(4)
Sn1 Sn1 2_656 4.0503(4)
Ga1 Cl2 . 2.2159(9)
Ga1 Cl3 . 2.1625(10)
Ga1 Cl4 . 2.1691(8)
Ga1 Cl5 . 2.1439(10)
C1 C2 . 1.379(5)
C1 C6 . 1.388(5)
C1 H1 . 0.9400
C2 C3 . 1.395(4)
C2 H2 . 0.9400
C3 C4 . 1.408(4)
C3 C7 . 1.503(4)
C4 C5 . 1.408(5)
C4 C8 . 1.505(5)
C5 C6 . 1.404(5)
C5 C9 . 1.517(5)
C6 C10 . 1.513(5)
C7 H71 . 0.9700
C7 H72 . 0.9700
C7 H73 . 0.9700
C8 H81 . 0.9700
C8 H82 . 0.9700
C8 H83 . 0.9700
C9 H91 . 0.9700
C9 H92 . 0.9700
C9 H93 . 0.9700
C10 H101 . 0.9700
C10 H102 . 0.9700
C10 H103 . 0.9700
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
C10 H103 Cl3 . 0.97 2.74 3.605(4) 149.4 yes
C7 H71 Cl4 2_666 0.97 2.78 3.612(4) 144.1 yes

_cod_database_fobs_code 2242994
