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#$Date: 2016-03-25 12:38:46 +0100 (vie 25 de mar de 2016) $
#$Revision: 179855 $
#$URL: svn://www.crystallography.net/cod/cif/7/01/51/7015127.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7015127
loop_
_publ_author_name
'Muesmann, Thomas W. T.'
'Zitzer, Christina'
'Mietrach, Andrea'
'Klüner, Thorsten'
'Christoffers, Jens'
'Wickleder, Mathias S.'
_publ_section_title
;
 para-Benzene disulfonic acid and its tetrachloro and tetrafluoro
 derivatives--studies towards polyhalogenated metal-organic-frameworks
 with sulfo analogues of terephthalic acid.
;
_journal_issue                   13
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              3128
_journal_page_last               3141
_journal_paper_doi               10.1039/c0dt01223h
_journal_volume                  40
_journal_year                    2011
_chemical_formula_sum            'C18 H28 Cl4 N4 O10 S2 Zn'
_chemical_formula_weight         731.73
_chemical_name_systematic
;
?
;
_space_group_IT_number           2
_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_creation_method           SHELXL-97
_cell_angle_alpha                91.409(16)
_cell_angle_beta                 106.723(16)
_cell_angle_gamma                90.440(16)
_cell_formula_units_Z            1
_cell_length_a                   9.0518(12)
_cell_length_b                   9.8960(10)
_cell_length_c                   8.3148(11)
_cell_measurement_temperature    293(2)
_cell_volume                     713.01(16)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.916
_diffrn_measured_fraction_theta_max 0.916
_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  0.0428
_diffrn_reflns_av_sigmaI/netI    0.0329
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            11246
_diffrn_reflns_theta_full        28.28
_diffrn_reflns_theta_max         28.28
_diffrn_reflns_theta_min         2.93
_exptl_absorpt_coefficient_mu    1.440
_exptl_crystal_density_diffrn    1.704
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             374
_refine_diff_density_max         0.498
_refine_diff_density_min         -0.451
_refine_diff_density_rms         0.061
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.755
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     234
_refine_ls_number_reflns         3226
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.755
_refine_ls_R_factor_all          0.0323
_refine_ls_R_factor_gt           0.0257
_refine_ls_shift/su_max          1.273
_refine_ls_shift/su_mean         0.321
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0000P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0495
_refine_ls_wR_factor_ref         0.0501
_reflns_number_gt                2699
_reflns_number_total             3226
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c0dt01223h.txt
_cod_data_source_block           c:\cz12\cz12_neu\cz12
_cod_original_cell_volume        713.01(15)
_cod_database_code               7015127
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Zn1 Zn 0.5000 0.5000 0.5000 0.01625(8) Uani 1 2 d S . .
S5 S 0.75254(4) 0.76343(5) 0.62601(5) 0.01732(10) Uani 1 1 d . . .
Cl1 Cl 0.50810(5) 0.83784(5) 0.81684(5) 0.02696(11) Uani 1 1 d . . .
Cl2 Cl 0.27259(6) 1.05158(7) 0.71297(7) 0.04387(16) Uani 1 1 d . . .
C6 C 0.50565(18) 0.92591(18) 0.6395(2) 0.0167(3) Uani 1 1 d . . .
O8 O 0.66397(13) 0.34963(14) 0.59619(15) 0.0237(3) Uani 1 1 d . . .
N8 N 0.78719(15) 0.19912(17) 0.78809(18) 0.0207(3) Uani 1 1 d . . .
O9 O 0.66022(13) 0.64522(13) 0.64166(14) 0.0199(3) Uani 1 1 d . . .
O10 O 0.58588(13) 0.52121(14) 0.29790(15) 0.0230(3) Uani 1 1 d . . .
O11 O 0.84281(13) 0.81684(14) 0.78745(16) 0.0267(3) Uani 1 1 d . . .
O12 O 0.83693(14) 0.74124(14) 0.50556(17) 0.0281(3) Uani 1 1 d . . .
C9 C 0.67749(19) 0.28612(19) 0.7260(2) 0.0197(4) Uani 1 1 d . . .
H1 H 0.601(2) 0.300(2) 0.789(3) 0.025(5) Uiso 1 1 d . . .
C7 C 0.39674(18) 1.02756(18) 0.5915(2) 0.0174(3) Uani 1 1 d . . .
C8 C 0.61121(17) 0.89507(18) 0.5495(2) 0.0152(3) Uani 1 1 d . . .
N9 N 0.78606(15) 0.51042(16) 0.18660(17) 0.0199(3) Uani 1 1 d . . .
C10 C 0.71749(19) 0.4838(2) 0.3025(2) 0.0236(4) Uani 1 1 d . . .
H2 H 0.784(2) 0.437(2) 0.402(3) 0.022(5) Uiso 1 1 d . . .
C11 C 0.7949(2) 0.1287(3) 0.9433(2) 0.0317(5) Uani 1 1 d . . .
H3 H 0.786(3) 0.030(3) 0.924(3) 0.032(6) Uiso 1 1 d . . .
H6 H 0.900(3) 0.157(3) 1.033(3) 0.051(7) Uiso 1 1 d . . .
H9 H 0.708(3) 0.157(3) 0.971(3) 0.051(7) Uiso 1 1 d . . .
C12 C 0.7131(2) 0.5950(3) 0.0473(3) 0.0336(5) Uani 1 1 d . . .
H7 H 0.784(4) 0.653(4) 0.017(4) 0.077(10) Uiso 1 1 d . . .
H11 H 0.717(5) 0.547(5) -0.041(6) 0.135(17) Uiso 1 1 d . . .
H12 H 0.614(5) 0.624(4) 0.034(5) 0.104(14) Uiso 1 1 d . . .
C13 C 0.9059(2) 0.1660(3) 0.7068(3) 0.0330(5) Uani 1 1 d . . .
H4 H 0.913(3) 0.070(3) 0.699(3) 0.034(6) Uiso 1 1 d . . .
H10 H 1.007(4) 0.193(3) 0.785(4) 0.064(9) Uiso 1 1 d . . .
H14 H 0.881(3) 0.209(3) 0.606(4) 0.063(9) Uiso 1 1 d . . .
C14 C 0.9415(2) 0.4635(3) 0.2018(3) 0.0388(5) Uani 1 1 d . . .
H5 H 0.971(3) 0.422(3) 0.297(4) 0.056(8) Uiso 1 1 d . . .
H8 H 0.941(3) 0.413(3) 0.095(4) 0.069(9) Uiso 1 1 d . . .
H13 H 1.013(3) 0.541(3) 0.208(4) 0.058(8) Uiso 1 1 d . . .
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'
O O 0.0106 0.0060 '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'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zn Zn 0.2839 1.4301 '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
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O10 Zn1 O10 180.0 . 2_666 ?
O10 Zn1 O9 90.93(5) . . ?
O10 Zn1 O9 89.07(5) 2_666 . ?
O10 Zn1 O9 89.07(5) . 2_666 ?
O10 Zn1 O9 90.93(5) 2_666 2_666 ?
O9 Zn1 O9 180.0 . 2_666 ?
O10 Zn1 O8 89.70(5) . 2_666 ?
O10 Zn1 O8 90.30(5) 2_666 2_666 ?
O9 Zn1 O8 91.73(5) . 2_666 ?
O9 Zn1 O8 88.27(5) 2_666 2_666 ?
O10 Zn1 O8 90.30(5) . . ?
O10 Zn1 O8 89.70(5) 2_666 . ?
O9 Zn1 O8 88.27(5) . . ?
O9 Zn1 O8 91.73(5) 2_666 . ?
O8 Zn1 O8 180.0 2_666 . ?
O12 S5 O11 115.06(8) . . ?
O12 S5 O9 112.48(8) . . ?
O11 S5 O9 111.92(7) . . ?
O12 S5 C8 108.57(7) . . ?
O11 S5 C8 103.28(8) . . ?
O9 S5 C8 104.49(7) . . ?
C8 C6 C7 122.27(14) . . ?
C8 C6 Cl1 120.11(13) . . ?
C7 C6 Cl1 117.62(12) . . ?
C9 O8 Zn1 126.36(12) . . ?
C9 N8 C13 122.50(16) . . ?
C9 N8 C11 121.15(15) . . ?
C13 N8 C11 116.34(17) . . ?
S5 O9 Zn1 142.79(7) . . ?
C10 O10 Zn1 121.57(11) . . ?
O8 C9 N8 124.76(16) . . ?
C8 C7 C6 121.11(14) 2_676 . ?
C8 C7 Cl2 122.06(13) 2_676 . ?
C6 C7 Cl2 116.83(12) . . ?
C7 C8 C6 116.62(15) 2_676 . ?
C7 C8 S5 124.48(12) 2_676 . ?
C6 C8 S5 118.86(12) . . ?
C10 N9 C12 120.76(15) . . ?
C10 N9 C14 120.86(16) . . ?
C12 N9 C14 118.25(16) . . ?
O10 C10 N9 124.21(16) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Zn1 O10 2.0588(11) . ?
Zn1 O10 2.0588(11) 2_666 ?
Zn1 O9 2.1113(13) . ?
Zn1 O9 2.1113(13) 2_666 ?
Zn1 O8 2.1133(13) 2_666 ?
Zn1 O8 2.1133(13) . ?
S5 O12 1.4377(13) . ?
S5 O11 1.4409(13) . ?
S5 O9 1.4625(12) . ?
S5 C8 1.8265(17) . ?
Cl1 C6 1.7259(16) . ?
Cl2 C7 1.7275(15) . ?
C6 C8 1.404(2) . ?
C6 C7 1.397(2) . ?
O8 C9 1.238(2) . ?
N8 C9 1.317(2) . ?
N8 C13 1.460(2) . ?
N8 C11 1.466(2) . ?
O10 C10 1.241(2) . ?
C7 C8 1.401(2) 2_676 ?
C8 C7 1.401(2) 2_676 ?
N9 C10 1.318(2) . ?
N9 C12 1.447(2) . ?
N9 C14 1.457(2) . ?
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
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O10 Zn1 O8 C9 -178.89(15) . . . . ?
O10 Zn1 O8 C9 1.11(15) 2_666 . . . ?
O9 Zn1 O8 C9 90.20(15) . . . . ?
O9 Zn1 O8 C9 -89.80(15) 2_666 . . . ?
O8 Zn1 O8 C9 -85(100) 2_666 . . . ?
O12 S5 O9 Zn1 -48.80(15) . . . . ?
O11 S5 O9 Zn1 179.85(11) . . . . ?
C8 S5 O9 Zn1 68.77(14) . . . . ?
O10 Zn1 O9 S5 26.69(13) . . . . ?
O10 Zn1 O9 S5 -153.31(13) 2_666 . . . ?
O9 Zn1 O9 S5 117(100) 2_666 . . . ?
O8 Zn1 O9 S5 -63.04(13) 2_666 . . . ?
O8 Zn1 O9 S5 116.96(13) . . . . ?
O10 Zn1 O10 C10 -42(100) 2_666 . . . ?
O9 Zn1 O10 C10 67.79(15) . . . . ?
O9 Zn1 O10 C10 -112.21(15) 2_666 . . . ?
O8 Zn1 O10 C10 159.51(16) 2_666 . . . ?
O8 Zn1 O10 C10 -20.49(16) . . . . ?
Zn1 O8 C9 N8 -175.47(13) . . . . ?
C13 N8 C9 O8 -1.1(3) . . . . ?
C11 N8 C9 O8 179.71(18) . . . . ?
C8 C6 C7 C8 -0.5(3) . . . 2_676 ?
Cl1 C6 C7 C8 179.07(13) . . . 2_676 ?
C8 C6 C7 Cl2 178.92(14) . . . . ?
Cl1 C6 C7 Cl2 -1.46(19) . . . . ?
C7 C6 C8 C7 0.5(3) . . . 2_676 ?
Cl1 C6 C8 C7 -179.09(13) . . . 2_676 ?
C7 C6 C8 S5 178.32(13) . . . . ?
Cl1 C6 C8 S5 -1.3(2) . . . . ?
O12 S5 C8 C7 -7.88(17) . . . 2_676 ?
O11 S5 C8 C7 114.69(15) . . . 2_676 ?
O9 S5 C8 C7 -128.11(15) . . . 2_676 ?
O12 S5 C8 C6 174.50(13) . . . . ?
O11 S5 C8 C6 -62.92(15) . . . . ?
O9 S5 C8 C6 54.28(15) . . . . ?
Zn1 O10 C10 N9 -170.75(14) . . . . ?
C12 N9 C10 O10 4.0(3) . . . . ?
C14 N9 C10 O10 179.6(2) . . . . ?
