#------------------------------------------------------------------------------
#$Date: 2018-07-21 16:52:05 +0300 (Sat, 21 Jul 2018) $
#$Revision: 209173 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/34/54/4345475.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_4345475
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            'C12 H14 Cu N2 O10 S'
_chemical_formula_weight         441.85
_space_group_crystal_system      monoclinic
_space_group_IT_number           12
_space_group_name_Hall           '-I 2y'
_space_group_name_H-M_alt        'I 1 2/m 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2016/4
_cell_angle_alpha                90.000(5)
_cell_angle_beta                 92.328(5)
_cell_angle_gamma                90.000(5)
_cell_formula_units_Z            4
_cell_length_a                   11.728(5)
_cell_length_b                   6.853(5)
_cell_length_c                   20.166(5)
_cell_measurement_reflns_used    250
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      2
_cell_volume                     1619.4(14)
_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 0.999
_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  0.0381
_diffrn_reflns_av_unetI/netI     0.0267
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            12386
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.528
_diffrn_reflns_theta_min         1.975
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    1.537
_exptl_absorpt_correction_T_max  0.9874
_exptl_absorpt_correction_T_min  0.8528
_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            Blue
_exptl_crystal_density_diffrn    1.812
_exptl_crystal_description       Needle
_exptl_crystal_F_000             900
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.132
_refine_diff_density_min         -0.550
_refine_diff_density_rms         0.089
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     167
_refine_ls_number_reflns         2020
_refine_ls_number_restraints     11
_refine_ls_restrained_S_all      1.062
_refine_ls_R_factor_all          0.0433
_refine_ls_R_factor_gt           0.0372
_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)+(0.0535P)²+3.4141P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0977
_refine_ls_wR_factor_ref         0.1018
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1780
_reflns_number_total             2020
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            ic6b02674_si_002.cif
_cod_data_source_block           DG-2
_cod_depositor_comments
;
 Updating space group information.

 Antanas Vaitkus,
 2018-07-22
;
_cod_original_sg_symbol_H-M      'I 2/m'
_cod_database_code               4345475
_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_id
_space_group_symop_operation_xyz
1 'x, y, z'
2 '-x, y, -z'
3 'x+1/2, y+1/2, z+1/2'
4 '-x+1/2, y+1/2, -z+1/2'
5 '-x, -y, -z'
6 'x, -y, z'
7 '-x+1/2, -y+1/2, -z+1/2'
8 '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
CU1 Cu 0.27722(3) 0.000000 0.47511(2) 0.02375(15) Uani 1 2 d DS T P
S1 S 0.51916(8) 0.000000 0.84576(5) 0.0337(2) Uani 1 2 d S T P
O2 O 0.4265(2) 0.000000 0.57961(13) 0.0460(8) Uani 1 2 d S T P
O1W O 0.3568(2) 0.000000 0.38987(13) 0.0366(6) Uani 1 2 d DS T P
O1 O 0.2393(2) 0.000000 0.56841(12) 0.0279(5) Uani 1 2 d S T P
N1 N 0.28374(16) 0.2980(3) 0.47744(9) 0.0251(4) Uani 1 1 d . . .
O3 O 0.6186(3) 0.000000 0.80745(18) 0.0662(11) Uani 1 2 d S T P
O4 O 0.5039(2) 0.1710(4) 0.88615(13) 0.0661(8) Uani 1 1 d . . .
C1 C 0.3299(3) 0.000000 0.60377(17) 0.0283(7) Uani 1 2 d S T P
C3 C 0.2090(3) 0.000000 0.70297(16) 0.0225(6) Uani 1 2 d S T P
H3 H 0.144839 0.000000 0.674330 0.027 Uiso 1 2 calc R U P
O2W O 0.1110(3) 0.000000 0.4261(2) 0.0625(11) Uani 1 2 d DS T P
C8 C 0.0832(3) 0.000000 0.8012(2) 0.0424(10) Uani 1 2 d S T P
C6 C 0.4003(3) 0.000000 0.78845(16) 0.0236(7) Uani 1 2 d S T P
C4 C 0.1971(3) 0.000000 0.77134(17) 0.0254(7) Uani 1 2 d S T P
C10 C 0.1982(2) 0.3987(4) 0.50234(12) 0.0276(5) Uani 1 1 d . . .
H10 H 0.137345 0.332112 0.520023 0.033 Uiso 1 1 calc R U .
C5 C 0.2927(3) 0.000000 0.81374(17) 0.0262(7) Uani 1 2 d S T P
H5 H 0.284533 0.000000 0.859418 0.031 Uiso 1 2 calc R U P
C9 C 0.3703(2) 0.3989(4) 0.45377(13) 0.0304(5) Uani 1 1 d . . .
H9 H 0.431921 0.332384 0.436935 0.036 Uiso 1 1 calc R U .
O5 O 0.0714(3) 0.000000 0.85988(17) 0.0801(15) Uani 1 2 d S T P
C7 C 0.4129(3) 0.000000 0.72088(17) 0.0288(7) Uani 1 2 d S T P
H7 H 0.485519 0.000000 0.704042 0.035 Uiso 1 2 calc R U P
O6 O -0.0019(3) 0.000000 0.75721(17) 0.0674(12) Uani 1 2 d S T P
H6 H -0.058555 -0.046614 0.773714 0.101 Uiso 0.5 1 calc R U P
C2 C 0.3177(3) 0.000000 0.67781(16) 0.0244(7) Uani 1 2 d S T P
O3W O 0.3085(4) 0.2608(9) 0.2947(3) 0.0561(13) Uani 0.5 1 d D . P
H1WB H 0.428(2) 0.02(2) 0.393(2) 0.084 Uiso 0.5 1 d D U P
H1WA H 0.325(4) 0.058(10) 0.3574(19) 0.084 Uiso 0.5 1 d D U P
H2WA H 0.087(5) -0.092(7) 0.401(4) 0.084 Uiso 0.5 1 d D U P
H2WB H 0.072(4) 0.099(5) 0.419(4) 0.084 Uiso 0.5 1 d D U P
H3WB H 0.261(6) 0.168(8) 0.285(5) 0.084 Uiso 0.5 1 d D U P
H3WA H 0.268(6) 0.364(7) 0.298(5) 0.084 Uiso 0.5 1 d D U 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'
Cu Cu 0.3201 1.2651 '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'
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 CU1 O1W 165.19(11) . .
O1 CU1 N1 89.29(5) . .
O1W CU1 N1 90.08(5) . .
O1 CU1 N1 89.29(5) . 6
O1W CU1 N1 90.08(5) . 6
N1 CU1 N1 175.06(11) . 6
O1 CU1 O2W 101.84(15) . .
O1W CU1 O2W 92.97(16) . .
N1 CU1 O2W 92.46(5) . .
N1 CU1 O2W 92.46(6) 6 .
O3 S1 O4 115.42(13) . 6
O3 S1 O4 115.42(14) . .
O4 S1 O4 108.7(3) 6 .
O3 S1 C6 106.59(19) . .
O4 S1 C6 104.80(13) 6 .
O4 S1 C6 104.80(13) . .
C1 O1 CU1 109.1(2) . .
C9 N1 C10 117.5(2) . .
C9 N1 CU1 122.59(17) . .
C10 N1 CU1 119.87(17) . .
O2 C1 O1 122.5(3) . .
O2 C1 C2 120.7(3) . .
O1 C1 C2 116.8(3) . .
C2 C3 C4 119.5(3) . .
O5 C8 O6 123.7(4) . .
O5 C8 C4 122.9(4) . .
O6 C8 C4 113.4(3) . .
C7 C6 C5 120.1(3) . .
C7 C6 S1 122.1(3) . .
C5 C6 S1 117.7(3) . .
C5 C4 C3 120.1(3) . .
C5 C4 C8 117.9(3) . .
C3 C4 C8 122.0(3) . .
N1 C10 C10 121.19(15) . 6_565
C6 C5 C4 120.2(3) . .
N1 C9 C9 121.26(14) . 6_565
C6 C7 C2 120.3(3) . .
C7 C2 C3 119.9(3) . .
C7 C2 C1 121.0(3) . .
C3 C2 C1 119.2(3) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
CU1 O1 1.951(2) .
CU1 O1W 1.989(3) .
CU1 N1 2.044(3) .
CU1 N1 2.044(3) 6
CU1 O2W 2.149(3) .
S1 O3 1.425(3) .
S1 O4 1.443(3) 6
S1 O4 1.443(3) .
S1 C6 1.774(3) .
O2 C1 1.251(4) .
O1 C1 1.255(4) .
N1 C9 1.333(3) .
N1 C10 1.333(3) .
C1 C2 1.506(5) .
C3 C2 1.391(5) .
C3 C4 1.391(5) .
C8 O5 1.197(5) .
C8 O6 1.309(5) .
C8 C4 1.487(5) .
C6 C7 1.377(5) .
C6 C5 1.380(5) .
C4 C5 1.383(5) .
C10 C10 1.388(5) 6_565
C9 C9 1.385(5) 6_565
C7 C2 1.386(5) .
