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#$Date: 2017-03-04 04:16:38 +0200 (Sat, 04 Mar 2017) $
#$Revision: 192997 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/34/54/4345478.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_4345478
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            'C36 H30 Cu N4 O20 S2'
_chemical_formula_weight         966.30
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2016/4
_cell_angle_alpha                90
_cell_angle_beta                 112.858(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.8191(4)
_cell_length_b                   11.0557(4)
_cell_length_c                   22.3316(7)
_cell_measurement_reflns_used    250
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      27.6
_cell_measurement_theta_min      2.0
_cell_volume                     4053.9(2)
_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 1.000
_diffrn_measured_fraction_theta_max 0.997
_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  0.0387
_diffrn_reflns_av_unetI/netI     0.0296
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            27710
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.591
_diffrn_reflns_theta_min         1.979
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.731
_exptl_absorpt_correction_T_max  0.9654
_exptl_absorpt_correction_T_min  0.8965
_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            Violet
_exptl_crystal_density_diffrn    1.583
_exptl_crystal_description       Block
_exptl_crystal_F_000             1980
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         2.046
_refine_diff_density_min         -2.171
_refine_diff_density_rms         0.117
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     305
_refine_ls_number_reflns         4698
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.1482
_refine_ls_R_factor_gt           0.1073
_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)+(0.0843P)²+58.2114P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2472
_refine_ls_wR_factor_ref         0.2782
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3166
_reflns_number_total             4698
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            ic6b02674_si_002.cif
_cod_data_source_block           DG5_rev
_cod_database_code               4345478
_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+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_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
_atom_site_refinement_flags_occupancy
C1 C 0.5517(4) 0.2697(8) 0.7312(3) 0.059(2) Uani 1 1 d . . .
H1 H 0.588112 0.228158 0.718127 0.071 Uiso 1 1 calc R U .
C2 C 0.5531(4) 0.3947(8) 0.7305(3) 0.0555(18) Uani 1 1 d . . .
H2 H 0.589676 0.434811 0.717018 0.067 Uiso 1 1 calc R U .
C3 C 0.500000 0.4608(11) 0.750000 0.055(3) Uani 1 2 d S T P
C4 C 0.500000 0.5934(10) 0.750000 0.051(2) Uani 1 2 d S T P
C5 C 0.4282(4) 0.6588(9) 0.7277(3) 0.067(2) Uani 1 1 d . . .
H5 H 0.378388 0.618861 0.712863 0.081 Uiso 1 1 calc R U .
C6 C 0.4308(5) 0.7842(8) 0.7274(3) 0.0610(18) Uani 1 1 d . . .
H6 H 0.382237 0.827504 0.710786 0.073 Uiso 1 1 calc R U .
C7 C 0.5619(4) -0.0343(6) 0.6475(3) 0.0514(16) Uani 1 1 d . . .
H7 H 0.604169 -0.069577 0.682176 0.062 Uiso 1 1 calc R U .
C8 C 0.5639(4) -0.0416(6) 0.5861(3) 0.0475(15) Uani 1 1 d . . .
H8 H 0.607995 -0.077465 0.580642 0.057 Uiso 1 1 calc R U .
C9 C 0.5005(4) 0.0043(6) 0.5336(2) 0.0460(15) Uani 1 1 d . . .
C10 C 0.4394(4) 0.0647(10) 0.5465(3) 0.079(3) Uani 1 1 d . . .
H10 H 0.396070 0.100336 0.512890 0.095 Uiso 1 1 calc R U .
C11 C 0.4438(4) 0.0712(10) 0.6097(3) 0.077(3) Uani 1 1 d . . .
H11 H 0.403273 0.113178 0.617444 0.093 Uiso 1 1 calc R U .
C12 C -0.0283(4) 0.1820(7) 0.5288(4) 0.0575(17) Uani 1 1 d . . .
C13 C 0.0567(4) 0.1381(6) 0.5421(3) 0.0479(15) Uani 1 1 d . . .
C14 C 0.1105(4) 0.1137(6) 0.6041(3) 0.0494(15) Uani 1 1 d . . .
H14 H 0.094359 0.121779 0.638802 0.059 Uiso 1 1 calc R U .
C15 C 0.1898(4) 0.0766(6) 0.6149(3) 0.0503(15) Uani 1 1 d . . .
C16 C 0.2127(4) 0.0638(7) 0.5635(4) 0.0577(18) Uani 1 1 d . . .
H16 H 0.265102 0.037531 0.570735 0.069 Uiso 1 1 calc R U .
C17 C 0.1601(4) 0.0891(8) 0.5023(4) 0.067(2) Uani 1 1 d . . .
C18 C 0.0813(4) 0.1272(8) 0.4911(3) 0.0629(19) Uani 1 1 d . . .
H18 H 0.045322 0.145288 0.449044 0.076 Uiso 1 1 calc R U .
C19 C 0.1910(8) 0.0712(17) 0.4506(5) 0.137(7) Uani 1 1 d . . .
N1 N 0.500000 0.2043(8) 0.750000 0.0499(19) Uani 1 2 d S T P
N2 N 0.500000 0.8430(9) 0.750000 0.054(2) Uani 1 2 d S T P
N3 N 0.5026(3) 0.0207(6) 0.6594(2) 0.0507(14) Uani 1 1 d . . .
O1 O -0.0741(3) 0.2122(7) 0.4756(3) 0.0861(19) Uani 1 1 d . . .
O2 O -0.0459(3) 0.1834(6) 0.5806(3) 0.0719(15) Uani 1 1 d . . .
O1W O 0.6825(4) 0.2105(9) 0.4358(4) 0.122(3) Uani 1 1 d G . .
O3 O 0.1516(5) 0.1281(11) 0.3978(4) 0.145(4) Uani 1 1 d . . .
O2W O 0.7166(5) 0.2081(12) 0.6260(4) 0.138(4) Uani 1 1 d G . .
H2WA H 0.666824 0.205112 0.600294 0.208 Uiso 1 1 d G U .
H2WB H 0.745298 0.230309 0.605140 0.208 Uiso 1 1 d G U .
O4 O 0.2539(7) -0.0097(11) 0.4640(5) 0.059(3) Uani 0.5 1 d . . P
O3W O 0.2504(7) 0.400(2) 0.6658(4) 0.268(10) Uani 1 1 d G . .
H3WA H 0.261296 0.475196 0.672001 0.402 Uiso 1 1 d G U .
H3WB H 0.255874 0.366990 0.701598 0.402 Uiso 1 1 d G U .
O4A O 0.2468(13) 0.078(3) 0.4449(9) 0.165(11) Uani 0.5 1 d . . P
O5 O 0.2514(4) 0.1478(8) 0.7363(3) 0.103(2) Uani 1 1 d . . .
O6 O 0.3405(3) 0.0448(6) 0.6951(3) 0.0796(19) Uani 1 1 d . . .
O7 O 0.2345(4) -0.0670(7) 0.7130(3) 0.100(2) Uani 1 1 d . . .
S1 S 0.26042(11) 0.0482(2) 0.69654(10) 0.0707(7) Uani 1 1 d . . .
CU1 Cu 0.500000 0.02531(13) 0.750000 0.0586(4) Uani 1 2 d S T P
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'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.3201 1.2651 '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
N1 C1 C2 123.6(7) . .
C1 C2 C3 120.2(7) . .
C2 C3 C2 116.7(11) . 2_656
C2 C3 C4 121.6(5) . .
C2 C3 C4 121.6(5) 2_656 .
C5 C4 C5 116.9(11) . 2_656
C5 C4 C3 121.5(5) . .
C5 C4 C3 121.5(5) 2_656 .
C4 C5 C6 119.8(8) . .
N2 C6 C5 121.4(8) . .
N3 C7 C8 123.3(6) . .
C9 C8 C7 119.7(6) . .
C8 C9 C10 116.6(5) . .
C8 C9 C9 121.3(7) . 5_656
C10 C9 C9 122.0(7) . 5_656
C11 C10 C9 119.6(7) . .
N3 C11 C10 123.2(7) . .
O1 C12 O2 124.6(7) . .
O1 C12 C13 122.0(7) . .
O2 C12 C13 113.4(6) . .
C14 C13 C18 119.7(6) . .
C14 C13 C12 121.2(6) . .
C18 C13 C12 119.0(6) . .
C13 C14 C15 119.8(6) . .
C16 C15 C14 119.7(6) . .
C16 C15 S1 121.0(5) . .
C14 C15 S1 119.3(5) . .
C17 C16 C15 120.8(6) . .
C16 C17 C18 119.9(7) . .
C16 C17 C19 116.2(9) . .
C18 C17 C19 123.9(9) . .
C13 C18 C17 120.1(7) . .
O4A C19 O3 93.4(18) . .
O4A C19 O4 49.0(19) . .
O3 C19 O4 129.2(10) . .
O4A C19 C17 138.0(15) . .
O3 C19 C17 114.7(13) . .
O4 C19 C17 116.0(13) . .
C1 N1 C1 115.7(10) . 2_656
C1 N1 CU1 122.2(5) . .
C1 N1 CU1 122.2(5) 2_656 .
C6 N2 C6 120.5(10) 2_656 .
C6 N2 CU1 119.7(5) 2_656 1_565
C6 N2 CU1 119.7(5) . 1_565
C11 N3 C7 117.3(5) . .
C11 N3 CU1 120.4(5) . .
C7 N3 CU1 122.2(4) . .
C19 O3 O4A 38.1(9) . .
O4A O4 C19 49.3(13) . .
O4 O4A C19 82(3) . .
O4 O4A O3 119(2) . .
C19 O4A O3 48.5(14) . .
O6 S1 O7 113.4(4) . .
O6 S1 O5 112.1(4) . .
O7 S1 O5 112.8(5) . .
O6 S1 C15 107.0(3) . .
O7 S1 C15 104.1(4) . .
O5 S1 C15 106.7(4) . .
N1 CU1 N2 180.0 . 1_545
N1 CU1 N3 91.41(18) . 2_656
N2 CU1 N3 88.59(18) 1_545 2_656
N1 CU1 N3 91.41(18) . .
N2 CU1 N3 88.59(18) 1_545 .
N3 CU1 N3 177.2(4) 2_656 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C1 N1 1.360(8) .
C1 C2 1.382(11) .
C2 C3 1.392(9) .
C3 C2 1.392(9) 2_656
C3 C4 1.466(15) .
C4 C5 1.383(9) .
C4 C5 1.383(9) 2_656
C5 C6 1.387(12) .
C6 N2 1.310(9) .
C7 N3 1.332(9) .
C7 C8 1.387(8) .
C8 C9 1.371(9) .
C9 C10 1.401(10) .
C9 C9 1.496(10) 5_656
C10 C11 1.383(9) .
C11 N3 1.318(10) .
C12 O1 1.199(9) .
C12 O2 1.310(9) .
C12 C13 1.506(9) .
C13 C14 1.370(9) .
C13 C18 1.377(10) .
C14 C15 1.400(8) .
C15 C16 1.367(10) .
C15 S1 1.794(7) .
C16 C17 1.354(11) .
C17 C18 1.391(10) .
C17 C19 1.473(12) .
C19 O4A 1.05(2) .
C19 O3 1.279(18) .
C19 O4 1.37(2) .
N1 C1 1.360(8) 2_656
N1 CU1 1.978(9) .
N2 C6 1.310(9) 2_656
N2 CU1 2.016(10) 1_565
N3 CU1 2.043(4) .
O3 O4A 1.70(2) .
O4 O4A 1.05(3) .
O5 S1 1.462(7) .
O6 S1 1.441(5) .
O7 S1 1.450(7) .
CU1 N2 2.016(10) 1_545
CU1 N3 2.043(4) 2_656
