#------------------------------------------------------------------------------
#$Date: 2016-02-20 22:30:07 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176789 $
#$URL: svn://www.crystallography.net/cod/cif/2/22/93/2229344.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_2229344
loop_
_publ_author_name
'Xiao, Wenzhi'
'Xue, Ruiting'
'Yin, Yansheng'
_publ_section_title
;
 Tetrakis[(4-methoxycarbonyl)anilinium] hexachloridostannate(IV)
 dichloride
;
_journal_coeditor_code           CV5035
_journal_issue                   3
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m297
_journal_paper_doi               10.1107/S1600536811003692
_journal_volume                  67
_journal_year                    2011
_chemical_formula_iupac          '(C8 H10 N O2)4 [Sn Cl6] Cl2'
_chemical_formula_moiety         '4(C8 H10 N O2 +), Cl6 Sn 2-, 2(Cl -)'
_chemical_formula_sum            'C32 H40 Cl8 N4 O8 Sn'
_chemical_formula_weight         1010.97
_chemical_name_systematic
;
Tetrakis[(4-methoxycarbonyl)anilinium] hexachloridostannate(IV) dichloride
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 119.424(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   30.748(3)
_cell_length_b                   7.1172(8)
_cell_length_c                   22.113(2)
_cell_measurement_reflns_used    4623
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      27.705
_cell_measurement_theta_min      2.721
_cell_volume                     4215.0(7)
_computing_cell_refinement       'SAINT (Bruker, 2007)'
_computing_data_collection       'SMART (Bruker, 2007)'
_computing_data_reduction        'SAINT (Bruker, 2007)'
_computing_molecular_graphics    'XP in SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker SMART CCD area-detector'
_diffrn_measurement_method       'φ and ω'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0349
_diffrn_reflns_av_sigmaI/netI    0.0389
_diffrn_reflns_limit_h_max       36
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            10221
_diffrn_reflns_theta_full        25.02
_diffrn_reflns_theta_max         25.02
_diffrn_reflns_theta_min         1.52
_exptl_absorpt_coefficient_mu    1.164
_exptl_absorpt_correction_T_max  0.6165
_exptl_absorpt_correction_T_min  0.5937
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.593
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2040
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.46
_exptl_crystal_size_min          0.46
_refine_diff_density_max         0.511
_refine_diff_density_min         -0.435
_refine_ls_extinction_coef       0.00204(13)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL97 (Sheldrick, 2008)'
_refine_ls_goodness_of_fit_ref   1.007
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     245
_refine_ls_number_reflns         3719
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.007
_refine_ls_R_factor_all          0.0473
_refine_ls_R_factor_gt           0.0307
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0450P)²+5.2918P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0739
_refine_ls_wR_factor_ref         0.0898
_reflns_number_gt                2969
_reflns_number_total             3719
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            cv5035.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               2229344
_cod_database_fobs_code          2229344
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'
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_disorder_assembly
_atom_site_disorder_group
Sn Sn1 0.0000 0.88525(4) 0.2500 0.03147(14) Uani d S 1 . .
Cl Cl1 0.05414(3) 1.12542(12) 0.24657(5) 0.0448(2) Uani d . 1 . .
Cl Cl2 0.04668(3) 0.88401(13) 0.37614(4) 0.0446(2) Uani d . 1 . .
Cl Cl3 0.05329(3) 0.64043(12) 0.24497(5) 0.0452(2) Uani d . 1 . .
Cl Cl4 0.01937(4) 0.27991(19) 0.05504(6) 0.0745(4) Uani d . 1 . .
N N1 0.05296(13) 0.8682(5) 0.09640(19) 0.0681(11) Uani d . 1 . .
H H1A 0.0488 0.8145 0.1295 0.102 Uiso calc R 1 . .
H H1B 0.0354 0.8058 0.0568 0.102 Uiso calc R 1 . .
H H1C 0.0425 0.9868 0.0908 0.102 Uiso calc R 1 . .
O O1 0.28945(11) 0.8266(5) 0.23899(19) 0.0801(9) Uani d . 1 . .
O O2 0.27319(15) 0.8654(6) 0.1308(2) 0.1100(15) Uani d . 1 . .
C C1 0.25910(17) 0.8534(6) 0.1724(3) 0.0614(12) Uani d . 1 . .
C C2 0.20539(15) 0.8609(5) 0.1534(2) 0.0488(9) Uani d . 1 . .
C C3 0.19023(15) 0.8011(7) 0.1997(2) 0.0596(11) Uani d . 1 . .
H H3 0.2138 0.7596 0.2437 0.071 Uiso calc R 1 . .
C C4 0.14066(15) 0.8028(7) 0.1808(2) 0.0627(12) Uani d . 1 . .
H H4 0.1305 0.7621 0.2119 0.075 Uiso calc R 1 . .
C C5 0.10627(15) 0.8642(5) 0.1165(2) 0.0510(10) Uani d . 1 . .
C C6 0.12064(16) 0.9276(6) 0.0699(2) 0.0563(10) Uani d . 1 . .
H H6 0.0971 0.9721 0.0265 0.068 Uiso calc R 1 . .
C C7 0.17023(16) 0.9236(6) 0.0889(2) 0.0571(11) Uani d . 1 . .
H H7 0.1803 0.9640 0.0577 0.069 Uiso calc R 1 . .
C C8 0.34155(17) 0.8066(9) 0.2610(3) 0.0977(18) Uani d . 1 . .
H H8A 0.3466 0.6959 0.2404 0.146 Uiso calc R 1 . .
H H8B 0.3601 0.7958 0.3107 0.146 Uiso calc R 1 . .
H H8C 0.3528 0.9148 0.2467 0.146 Uiso calc R 1 . .
N N2 -0.04641(12) 0.3799(4) 0.12080(17) 0.0549(8) Uani d . 1 . .
H H2A -0.0469 0.2835 0.1461 0.082 Uiso calc R 1 . .
H H2B -0.0329 0.4794 0.1481 0.082 Uiso calc R 1 . .
H H2C -0.0284 0.3495 0.1008 0.082 Uiso calc R 1 . .
O O3 -0.27704(11) 0.5652(5) -0.06223(17) 0.0754(9) Uani d . 1 . .
O O4 -0.25318(15) 0.6482(7) -0.1379(2) 0.1235(17) Uani d . 1 . .
C C9 -0.24390(17) 0.5845(7) -0.0834(2) 0.0649(12) Uani d . 1 . .
C C10 -0.19295(13) 0.5235(6) -0.03008(18) 0.0475(9) Uani d . 1 . .
C C11 -0.15324(15) 0.5639(6) -0.0409(2) 0.0530(10) Uani d . 1 . .
H H11 -0.1591 0.6244 -0.0814 0.064 Uiso calc R 1 . .
C C12 -0.10518(13) 0.5155(5) 0.00777(19) 0.0460(9) Uani d . 1 . .
H H12 -0.0785 0.5435 0.0007 0.055 Uiso calc R 1 . .
C C13 -0.09772(13) 0.4248(5) 0.06700(18) 0.0412(8) Uani d . 1 . .
C C14 -0.13659(14) 0.3806(5) 0.07820(19) 0.0484(9) Uani d . 1 . .
H H14 -0.1306 0.3179 0.1185 0.058 Uiso calc R 1 . .
C C15 -0.18453(14) 0.4296(6) 0.0293(2) 0.0538(10) Uani d . 1 . .
H H15 -0.2112 0.3995 0.0363 0.065 Uiso calc R 1 . .
C C16 -0.32747(17) 0.6233(8) -0.1111(3) 0.100(2) Uani d . 1 . .
H H16A -0.3402 0.5467 -0.1521 0.150 Uiso calc R 1 . .
H H16B -0.3274 0.7526 -0.1234 0.150 Uiso calc R 1 . .
H H16C -0.3483 0.6091 -0.0903 0.150 Uiso calc R 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'
O O 0.0106 0.0060 '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_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
Cl1 Sn1 Cl1 . 2 89.79(5) ?
Cl1 Sn1 Cl2 . 2 89.66(3) ?
Cl1 Sn1 Cl2 2 2 90.63(3) ?
Cl1 Sn1 Cl2 . . 90.63(3) ?
Cl1 Sn1 Cl2 2 . 89.66(3) ?
Cl2 Sn1 Cl2 2 . 179.58(4) ?
Cl1 Sn1 Cl3 . . 90.88(3) ?
Cl1 Sn1 Cl3 2 . 179.00(3) ?
Cl2 Sn1 Cl3 2 . 88.64(3) ?
Cl2 Sn1 Cl3 . . 91.06(3) ?
Cl1 Sn1 Cl3 . 2 179.00(3) ?
Cl1 Sn1 Cl3 2 2 90.88(3) ?
Cl2 Sn1 Cl3 2 2 91.06(3) ?
Cl2 Sn1 Cl3 . 2 88.64(3) ?
Cl3 Sn1 Cl3 . 2 88.45(4) ?
C5 N1 H1A . . 109.5 ?
C5 N1 H1B . . 109.5 ?
H1A N1 H1B . . 109.5 ?
C5 N1 H1C . . 109.5 ?
H1A N1 H1C . . 109.5 ?
H1B N1 H1C . . 109.5 ?
C1 O1 C8 . . 117.0(4) ?
O2 C1 O1 . . 123.1(4) ?
O2 C1 C2 . . 123.4(5) ?
O1 C1 C2 . . 113.5(4) ?
C7 C2 C3 . . 119.2(4) ?
C7 C2 C1 . . 120.1(4) ?
C3 C2 C1 . . 120.6(4) ?
C4 C3 C2 . . 120.1(4) ?
C4 C3 H3 . . 120.0 ?
C2 C3 H3 . . 120.0 ?
C5 C4 C3 . . 119.9(4) ?
C5 C4 H4 . . 120.0 ?
C3 C4 H4 . . 120.0 ?
C4 C5 C6 . . 121.0(4) ?
C4 C5 N1 . . 119.9(3) ?
C6 C5 N1 . . 119.0(4) ?
C7 C6 C5 . . 118.8(4) ?
C7 C6 H6 . . 120.6 ?
C5 C6 H6 . . 120.6 ?
C6 C7 C2 . . 121.0(3) ?
C6 C7 H7 . . 119.5 ?
C2 C7 H7 . . 119.5 ?
O1 C8 H8A . . 109.5 ?
O1 C8 H8B . . 109.5 ?
H8A C8 H8B . . 109.5 ?
O1 C8 H8C . . 109.5 ?
H8A C8 H8C . . 109.5 ?
H8B C8 H8C . . 109.5 ?
C13 N2 H2A . . 109.5 ?
C13 N2 H2B . . 109.5 ?
H2A N2 H2B . . 109.5 ?
C13 N2 H2C . . 109.5 ?
H2A N2 H2C . . 109.5 ?
H2B N2 H2C . . 109.5 ?
C9 O3 C16 . . 115.8(4) ?
O4 C9 O3 . . 124.0(4) ?
O4 C9 C10 . . 123.4(5) ?
O3 C9 C10 . . 112.6(4) ?
C15 C10 C11 . . 119.7(3) ?
C15 C10 C9 . . 121.8(4) ?
C11 C10 C9 . . 118.5(4) ?
C12 C11 C10 . . 120.8(4) ?
C12 C11 H11 . . 119.6 ?
C10 C11 H11 . . 119.6 ?
C13 C12 C11 . . 118.3(3) ?
C13 C12 H12 . . 120.9 ?
C11 C12 H12 . . 120.9 ?
C14 C13 C12 . . 121.8(3) ?
C14 C13 N2 . . 119.2(3) ?
C12 C13 N2 . . 118.9(3) ?
C13 C14 C15 . . 119.5(4) ?
C13 C14 H14 . . 120.3 ?
C15 C14 H14 . . 120.3 ?
C14 C15 C10 . . 119.8(4) ?
C14 C15 H15 . . 120.1 ?
C10 C15 H15 . . 120.1 ?
O3 C16 H16A . . 109.5 ?
O3 C16 H16B . . 109.5 ?
H16A C16 H16B . . 109.5 ?
O3 C16 H16C . . 109.5 ?
H16A C16 H16C . . 109.5 ?
H16B C16 H16C . . 109.5 ?
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 Cl1 . 2.4131(8) ?
Sn1 Cl1 2 2.4131(8) ?
Sn1 Cl2 2 2.4305(9) ?
Sn1 Cl2 . 2.4305(9) ?
Sn1 Cl3 . 2.4315(8) ?
Sn1 Cl3 2 2.4315(8) ?
N1 C5 . 1.473(5) ?
N1 H1A . 0.8900 ?
N1 H1B . 0.8900 ?
N1 H1C . 0.8900 ?
O1 C1 . 1.314(6) ?
O1 C8 . 1.434(5) ?
O2 C1 . 1.197(5) ?
C1 C2 . 1.492(5) ?
C2 C7 . 1.373(6) ?
C2 C3 . 1.384(5) ?
C3 C4 . 1.368(5) ?
C3 H3 . 0.9300 ?
C4 C5 . 1.362(5) ?
C4 H4 . 0.9300 ?
C5 C6 . 1.380(5) ?
C6 C7 . 1.369(5) ?
C6 H6 . 0.9300 ?
C7 H7 . 0.9300 ?
C8 H8A . 0.9600 ?
C8 H8B . 0.9600 ?
C8 H8C . 0.9600 ?
N2 C13 . 1.471(4) ?
N2 H2A . 0.8900 ?
N2 H2B . 0.8900 ?
N2 H2C . 0.8900 ?
O3 C9 . 1.320(5) ?
O3 C16 . 1.448(5) ?
O4 C9 . 1.185(5) ?
C9 C10 . 1.489(5) ?
C10 C15 . 1.380(5) ?
C10 C11 . 1.384(5) ?
C11 C12 . 1.377(5) ?
C11 H11 . 0.9300 ?
C12 C13 . 1.375(5) ?
C12 H12 . 0.9300 ?
C13 C14 . 1.371(5) ?
C14 C15 . 1.378(5) ?
C14 H14 . 0.9300 ?
C15 H15 . 0.9300 ?
C16 H16A . 0.9600 ?
C16 H16B . 0.9600 ?
C16 H16C . 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
N1 H1A Cl3 . 0.89 2.78 3.659(4) 170
N2 H2B Cl3 . 0.89 2.71 3.479(3) 145
N2 H2C Cl4 . 0.89 2.21 3.098(4) 177
N1 H1B Cl4 5_565 0.89 2.29 3.155(4) 165
N1 H1C Cl4 1_565 0.89 2.22 3.092(4) 166
N2 H2A Cl1 1_545 0.89 3.01 3.482(3) 115
C3 H3 O4 8_566 0.93 2.39 3.148(6) 139
C15 H15 O2 3_445 0.93 2.38 3.130(5) 138
