#------------------------------------------------------------------------------
#$Date: 2017-03-04 04:16:38 +0200 (Sat, 04 Mar 2017) $
#$Revision: 192997 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/34/54/4345474.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_4345474
loop_
_publ_author_name
'Maity, Dilip Kumar'
'Otake, Kenichi'
'Ghosh, Saheli'
'Kitagawa, Hiroshi'
'Ghoshal, Debajyoti'
_publ_section_title
;
 Sulfonic Group Functionalized Mixed Ligand Coordination Polymers:
 Synthesis, Characterization, Water Sorption, and Proton Conduction
 Studies.
;
_journal_issue                   3
_journal_name_full               'Inorganic chemistry'
_journal_page_first              1581
_journal_page_last               1590
_journal_paper_doi               10.1021/acs.inorgchem.6b02674
_journal_volume                  56
_journal_year                    2017
_chemical_formula_sum            'C20 H20 N2 O9 S Zn'
_chemical_formula_weight         529.81
_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   mixed
_audit_creation_method           SHELXL-2016/4
_cell_angle_alpha                79.092(5)
_cell_angle_beta                 76.637(5)
_cell_angle_gamma                66.689(5)
_cell_formula_units_Z            2
_cell_length_a                   7.861(5)
_cell_length_b                   9.523(5)
_cell_length_c                   15.901(5)
_cell_measurement_reflns_used    250
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      2.3
_cell_volume                     1057.2(9)
_computing_cell_refinement       'SMART APEX II'
_computing_data_collection       'SMART APEX II (BRUKER,2010)'
_computing_data_reduction        'SAINT (BRUKER,2000)'
_computing_molecular_graphics    'Ortep-3v2 for windows (Farrugia,1997)'
_computing_publication_material  'PLATON (Spek, 2008)'
_computing_structure_refinement  'SHELXL-2016/4 (Sheldrick, 2016)'
_computing_structure_solution    'SHELXS-2016/4 (Sheldrick, 2016)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0239
_diffrn_reflns_av_unetI/netI     0.0239
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            18252
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.541
_diffrn_reflns_theta_min         2.343
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    1.318
_exptl_absorpt_correction_T_max  0.9542
_exptl_absorpt_correction_T_min  0.8564
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
'XPREP' - A PROGRAM DATA PREPARATION & RECIPROCAL 
SPACE EXPLORATION,
Bruker Analytical X-ray Systems, 1997
;
_exptl_crystal_colour            White
_exptl_crystal_density_diffrn    1.664
_exptl_crystal_description       Block
_exptl_crystal_F_000             544
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.285
_refine_diff_density_min         -0.373
_refine_diff_density_rms         0.066
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     362
_refine_ls_number_reflns         4850
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.059
_refine_ls_R_factor_all          0.0344
_refine_ls_R_factor_gt           0.0286
_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)+(0.0401P)²+0.4136P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0739
_refine_ls_wR_factor_ref         0.0769
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4262
_reflns_number_total             4850
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            ic6b02674_si_002.cif
_cod_data_source_block           DG-1
_cod_database_code               4345474
_shelx_shelxl_version_number     2016/4
_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.
;
loop_
_space_group_symop_operation_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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
ZN1 Zn 0.77815(3) 0.33307(2) 0.96339(2) 0.02696(8) Uani 1 1 d . .
S1 S 0.31703(7) 0.14219(5) 0.69340(3) 0.02848(11) Uani 1 1 d . .
O5 O 0.3374(2) 0.04165(17) 0.63050(9) 0.0414(4) Uani 1 1 d . .
O7 O 0.7021(2) -0.44673(15) 0.93262(9) 0.0392(4) Uani 1 1 d . .
O3 O 0.1317(2) 0.1838(2) 0.74757(9) 0.0463(4) Uani 1 1 d . .
O4 O 0.3677(3) 0.27295(18) 0.65674(11) 0.0525(4) Uani 1 1 d . .
O6 O 0.7286(3) -0.45668(17) 0.79205(9) 0.0471(4) Uani 1 1 d . .
N1 N 0.7982(2) 0.32176(18) 1.08894(9) 0.0271(3) Uani 1 1 d . .
C7 C 0.6781(3) -0.1392(2) 0.89653(11) 0.0218(3) Uani 1 1 d . .
C4 C 0.4740(3) 0.0299(2) 0.76639(10) 0.0234(3) Uani 1 1 d . .
C3 C 0.5222(3) 0.1045(2) 0.81873(11) 0.0244(4) Uani 1 1 d . .
C1 C 0.6913(3) 0.1004(2) 0.93475(11) 0.0243(4) Uani 1 1 d . .
C8 C 0.6936(3) -0.3862(2) 0.85475(11) 0.0247(4) Uani 1 1 d . .
N2 N 0.7907(3) 0.3852(2) 1.65853(12) 0.0417(5) Uani 1 1 d . .
C5 C 0.5354(3) -0.1288(2) 0.77572(11) 0.0234(4) Uani 1 1 d . .
C2 C 0.6283(2) 0.01990(19) 0.88283(11) 0.0217(3) Uani 1 1 d . .
C6 C 0.6353(2) -0.21425(19) 0.84210(10) 0.0213(3) Uani 1 1 d . .
C11 C 0.8746(3) 0.3131(2) 1.25293(11) 0.0313(4) Uani 1 1 d . .
C18 C 0.8124(4) 0.2450(3) 1.64602(15) 0.0453(5) Uani 1 1 d . .
C10 C 0.8862(3) 0.1822(2) 1.22302(12) 0.0327(4) Uani 1 1 d . .
C16 C 0.7717(3) 0.3330(3) 1.49917(13) 0.0406(5) Uani 1 1 d . .
C12 C 0.8235(4) 0.4481(3) 1.19887(14) 0.0446(6) Uani 1 1 d . .
C20 C 0.7534(4) 0.4764(3) 1.51433(15) 0.0467(6) Uani 1 1 d . .
C14 C 0.9155(3) 0.3111(3) 1.34145(12) 0.0406(5) Uani 1 1 d . .
H14A H 1.026323 0.221449 1.352100 0.049 Uiso 1 1 calc R U
H14B H 0.941543 0.401986 1.342814 0.049 Uiso 1 1 calc R U
C19 C 0.7633(4) 0.5004(3) 1.59504(16) 0.0460(6) Uani 1 1 d . .
C17 C 0.8034(4) 0.2156(3) 1.56704(15) 0.0446(5) Uani 1 1 d . .
C9 C 0.8486(3) 0.1905(2) 1.14120(12) 0.0282(4) Uani 1 1 d . .
C15 C 0.7519(4) 0.3072(4) 1.41166(14) 0.0594(8) Uani 1 1 d . .
H15A H 0.740087 0.208258 1.416528 0.071 Uiso 1 1 calc R U
H15B H 0.637396 0.385865 1.395144 0.071 Uiso 1 1 calc R U
C13 C 0.7852(4) 0.4496(2) 1.11836(14) 0.0433(6) Uani 1 1 d . .
O1 O 0.6519(2) 0.24382(15) 0.91114(10) 0.0375(3) Uani 1 1 d . .
O2 O 0.7803(2) 0.03010(15) 0.99422(9) 0.0335(3) Uani 1 1 d . .
O1W O 1.0542(2) 0.23822(18) 0.91537(11) 0.0358(3) Uani 1 1 d . .
O2W O 0.2792(4) 0.1291(3) 0.45347(15) 0.0716(7) Uani 1 1 d . .
H1WA H 1.067(4) 0.228(3) 0.8720(19) 0.045(8) Uiso 1 1 d . .
H1WB H 1.107(4) 0.155(4) 0.946(2) 0.065(9) Uiso 1 1 d . .
H5 H 0.506(3) -0.180(2) 0.7404(14) 0.033(6) Uiso 1 1 d . .
H3 H 0.480(3) 0.214(2) 0.8117(13) 0.026(5) Uiso 1 1 d . .
H7 H 0.742(3) -0.197(2) 0.9413(13) 0.028(5) Uiso 1 1 d . .
H9 H 0.860(3) 0.102(3) 1.1202(14) 0.029(5) Uiso 1 1 d . .
H10 H 0.931(3) 0.084(3) 1.2561(16) 0.047(7) Uiso 1 1 d . .
H12 H 0.817(4) 0.539(3) 1.2161(18) 0.060(8) Uiso 1 1 d . .
H20 H 0.736(4) 0.562(3) 1.4679(19) 0.064(8) Uiso 1 1 d . .
H13 H 0.754(4) 0.544(3) 1.0785(19) 0.062(8) Uiso 1 1 d . .
H18 H 0.827(4) 0.171(3) 1.6929(19) 0.061(8) Uiso 1 1 d . .
H19 H 0.753(4) 0.584(3) 1.6017(18) 0.051(8) Uiso 1 1 d . .
H17 H 0.814(4) 0.114(4) 1.5622(19) 0.067(9) Uiso 1 1 d . .
H2WA H 0.272(5) 0.107(4) 0.508(3) 0.081(11) Uiso 1 1 d . .
H2WB H 0.366(6) 0.091(5) 0.434(3) 0.086(15) Uiso 1 1 d . .
H2 H 0.796(4) 0.396(3) 1.708(2) 0.069(9) 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'
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'
Zn Zn 0.2839 1.4301 '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'
H H 0.0000 0.0000 '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
O1 ZN1 O7 112.52(7) . 1_565
O1 ZN1 O1W 106.53(8) . .
O7 ZN1 O1W 107.35(7) 1_565 .
O1 ZN1 N1 130.52(7) . .
O7 ZN1 N1 99.31(6) 1_565 .
O1W ZN1 N1 98.29(7) . .
O4 S1 O5 114.39(10) . .
O4 S1 O3 112.84(11) . .
O5 S1 O3 111.09(10) . .
O4 S1 C4 106.97(10) . .
O5 S1 C4 106.30(9) . .
O3 S1 C4 104.44(9) . .
C8 O7 ZN1 121.86(12) . 1_545
C9 N1 C13 117.53(16) . .
C9 N1 ZN1 123.51(12) . .
C13 N1 ZN1 118.33(13) . .
C6 C7 C2 120.32(15) . .
C5 C4 C3 120.42(15) . .
C5 C4 S1 120.61(13) . .
C3 C4 S1 118.78(14) . .
C4 C3 C2 120.04(16) . .
O2 C1 O1 123.21(16) . .
O2 C1 C2 121.54(16) . .
O1 C1 C2 115.21(15) . .
O6 C8 O7 125.21(17) . .
O6 C8 C6 119.83(16) . .
O7 C8 C6 114.96(15) . .
C18 N2 C19 121.8(2) . .
C4 C5 C6 119.86(15) . .
C3 C2 C7 119.46(15) . .
C3 C2 C1 119.62(15) . .
C7 C2 C1 120.90(15) . .
C7 C6 C5 119.64(16) . .
C7 C6 C8 120.67(15) . .
C5 C6 C8 119.69(15) . .
C12 C11 C10 117.44(17) . .
C12 C11 C14 120.28(19) . .
C10 C11 C14 122.28(19) . .
N2 C18 C17 120.4(2) . .
C11 C10 C9 119.81(18) . .
C20 C16 C17 118.06(19) . .
C20 C16 C15 120.4(2) . .
C17 C16 C15 121.5(2) . .
C11 C12 C13 120.1(2) . .
C19 C20 C16 120.0(2) . .
C15 C14 C11 111.01(18) . .
N2 C19 C20 119.9(2) . .
C18 C17 C16 119.8(2) . .
N1 C9 C10 122.69(18) . .
C14 C15 C16 112.94(19) . .
N1 C13 C12 122.43(19) . .
C1 O1 ZN1 113.53(12) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
ZN1 O1 1.9274(14) .
ZN1 O7 1.9362(17) 1_565
ZN1 O1W 2.013(2) .
ZN1 N1 2.0182(15) .
S1 O4 1.4351(18) .
S1 O5 1.4525(15) .
S1 O3 1.4541(18) .
S1 C4 1.7780(18) .
O7 C8 1.268(2) .
O7 ZN1 1.9361(16) 1_545
O6 C8 1.225(2) .
N1 C9 1.333(2) .
N1 C13 1.343(3) .
C7 C6 1.390(2) .
C7 C2 1.393(2) .
C4 C5 1.383(3) .
C4 C3 1.387(2) .
C3 C2 1.390(2) .
C1 O2 1.236(2) .
C1 O1 1.275(2) .
C1 C2 1.498(2) .
C8 C6 1.502(2) .
N2 C18 1.326(3) .
N2 C19 1.328(3) .
C5 C6 1.395(2) .
C11 C12 1.374(3) .
C11 C10 1.379(3) .
C11 C14 1.510(2) .
C18 C17 1.360(3) .
C10 C9 1.381(3) .
C16 C20 1.377(4) .
C16 C17 1.387(3) .
C16 C15 1.510(3) .
C12 C13 1.378(3) .
C20 C19 1.370(3) .
C14 C15 1.504(3) .
