#------------------------------------------------------------------------------
#$Date: 2016-03-24 02:52:30 +0200 (Thu, 24 Mar 2016) $
#$Revision: 179601 $
#$URL: svn://www.crystallography.net/cod/cif/4/50/65/4506519.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_4506519
loop_
_publ_author_name
'Paul, Mithun'
'Adarsh, N. N.'
'Dastidar, Parthasarathi'
_publ_section_title
;
 CuIICoordination Polymers Capable of Gelation and Selective
 SO4--2Separation
;
_journal_issue                   8
_journal_name_full               'Crystal Growth & Design'
_journal_page_first              4135
_journal_paper_doi               10.1021/cg300649e
_journal_volume                  12
_journal_year                    2012
_chemical_formula_moiety         'C18 H16 Cu N6 O9 S, O'
_chemical_formula_sum            'C18 H24 Cu N6 O10 S'
_chemical_formula_weight         580.03
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 97.436(11)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   6.5115(13)
_cell_length_b                   19.407(3)
_cell_length_c                   9.7353(17)
_cell_measurement_temperature    100(2)
_cell_volume                     1219.9(4)
_computing_cell_refinement       'Bruker Apex II'
_computing_data_collection       'Bruker Apex II'
_computing_data_reduction        SAINT
_computing_molecular_graphics    'Mercury 2.3, Ortep3v2'
_computing_publication_material  SHELXTL-97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 3
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker Apex II'
_diffrn_measurement_method       'phi-omega scan'
_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  0.0581
_diffrn_reflns_av_sigmaI/netI    0.0896
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            4931
_diffrn_reflns_theta_full        22.00
_diffrn_reflns_theta_max         22.00
_diffrn_reflns_theta_min         2.10
_exptl_absorpt_coefficient_mu    1.045
_exptl_absorpt_correction_T_max  0.9210
_exptl_absorpt_correction_T_min  0.7728
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.579
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             598
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.861
_refine_diff_density_min         -0.435
_refine_diff_density_rms         0.109
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.07(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     325
_refine_ls_number_reflns         2756
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.022
_refine_ls_R_factor_all          0.0698
_refine_ls_R_factor_gt           0.0642
_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)+(0.1000P)²+0.5058P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1551
_refine_ls_wR_factor_ref         0.1595
_reflns_number_gt                2508
_reflns_number_total             2756
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg300649e_si_003.cif
_cod_data_source_block           704a2_0m
_cod_original_sg_symbol_H-M      P2(1)
_cod_database_code               4506519
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -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
Cu1 Cu 1.50745(16) 1.10498(5) 0.15592(11) 0.0301(4) Uani 1 1 d .
S1 S 1.0598(4) 1.17983(14) -0.0496(3) 0.0375(7) Uani 1 1 d .
N1 N 1.4395(13) 1.0045(4) 0.1096(9) 0.037(2) Uani 1 1 d .
C2 C 1.2820(14) 0.9708(5) 0.1536(11) 0.035(3) Uani 1 1 d .
H2 H 1.2078 0.9924 0.2168 0.042 Uiso 1 1 calc R
C3 C 1.2245(16) 0.9053(5) 0.1090(11) 0.036(3) Uani 1 1 d .
C4 C 1.3365(16) 0.8727(5) 0.0160(12) 0.046(3) Uani 1 1 d .
H4 H 1.3024 0.8284 -0.0152 0.055 Uiso 1 1 calc R
C5 C 1.5008(16) 0.9079(6) -0.0296(12) 0.051(3) Uani 1 1 d .
H5 H 1.5813 0.8863 -0.0891 0.061 Uiso 1 1 calc R
C6 C 1.5441(16) 0.9728(6) 0.0119(12) 0.043(3) Uani 1 1 d .
H6 H 1.6465 0.9970 -0.0259 0.052 Uiso 1 1 calc R
N7 N 1.0621(13) 0.8668(4) 0.1565(9) 0.041(2) Uani 1 1 d .
H7 H 1.0433 0.8260 0.1225 0.049 Uiso 1 1 calc R
C8 C 0.9341(17) 0.8856(5) 0.2473(11) 0.034(3) Uani 1 1 d .
O9 O 0.9353(11) 0.9428(4) 0.2998(8) 0.0424(19) Uani 1 1 d .
N10 N 0.8034(13) 0.8334(4) 0.2733(9) 0.039(2) Uani 1 1 d .
H10 H 0.8175 0.7953 0.2301 0.047 Uiso 1 1 calc R
C11 C 0.6454(15) 0.8340(5) 0.3637(10) 0.031(2) Uani 1 1 d .
C12 C 0.635(2) 0.8827(6) 0.4656(13) 0.056(4) Uani 1 1 d .
H12 H 0.7352 0.9169 0.4809 0.067 Uiso 1 1 calc R
C13 C 0.478(3) 0.8804(7) 0.5426(15) 0.089(6) Uani 1 1 d .
H13 H 0.4673 0.9148 0.6078 0.107 Uiso 1 1 calc R
C14 C 0.330(2) 0.8276(7) 0.5273(14) 0.057(4) Uani 1 1 d .
H14 H 0.2245 0.8258 0.5829 0.068 Uiso 1 1 calc R
C15 C 0.3468(17) 0.7791(5) 0.4285(10) 0.036(3) Uani 1 1 d .
C16 C 0.5005(15) 0.7823(5) 0.3478(10) 0.034(3) Uani 1 1 d .
H16 H 0.5082 0.7488 0.2803 0.040 Uiso 1 1 calc R
N17 N 0.2056(13) 0.7233(4) 0.4020(9) 0.039(2) Uani 1 1 d .
H17 H 0.2094 0.7009 0.3261 0.046 Uiso 1 1 calc R
C18 C 0.0630(15) 0.7013(5) 0.4860(11) 0.030(3) Uani 1 1 d .
O19 O 0.0587(12) 0.7217(4) 0.6041(7) 0.0444(19) Uani 1 1 d .
N20 N -0.0636(13) 0.6530(5) 0.4263(9) 0.047(2) Uani 1 1 d .
H20 H -0.0353 0.6387 0.3473 0.056 Uiso 1 1 calc R
C21 C -0.2361(15) 0.6218(4) 0.4731(10) 0.030(2) Uani 1 1 d .
C22 C -0.2744(14) 0.6262(4) 0.6075(9) 0.029(3) Uani 1 1 d .
H22 H -0.1825 0.6500 0.6717 0.035 Uiso 1 1 calc R
N23 N -0.4474(11) 0.5959(5) 0.6491(8) 0.031(2) Uani 1 1 d .
C24 C -0.5789(18) 0.5633(5) 0.5543(13) 0.046(3) Uani 1 1 d .
H24 H -0.6963 0.5430 0.5819 0.056 Uiso 1 1 calc R
C25 C -0.5478(18) 0.5585(5) 0.4166(11) 0.043(3) Uani 1 1 d .
H25 H -0.6432 0.5360 0.3526 0.052 Uiso 1 1 calc R
C26 C -0.3768(16) 0.5870(5) 0.3778(10) 0.039(3) Uani 1 1 d .
H26 H -0.3518 0.5834 0.2861 0.047 Uiso 1 1 calc R
O27 O 1.5836(11) 1.2056(4) 0.1953(8) 0.0458(19) Uani 1 1 d .
O28 O 1.8483(10) 1.0759(3) 0.2014(8) 0.0429(19) Uani 1 1 d .
O29 O 1.5418(10) 1.1232(3) -0.0406(7) 0.0387(19) Uani 1 1 d .
O30 O 0.9609(16) 1.2407(5) 0.0019(11) 0.083(3) Uani 1 1 d .
O31 O 1.1442(10) 1.1372(4) 0.0671(7) 0.0388(17) Uani 1 1 d .
O32 O 0.9064(14) 1.1440(6) -0.1406(8) 0.077(3) Uani 1 1 d .
O33 O 1.2246(11) 1.2028(4) -0.1279(8) 0.048(2) Uani 1 1 d .
O34 O 0.234(2) 0.2897(5) 0.2235(13) 0.100(4) Uani 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'
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
O29 Cu1 N23 173.0(3) . 2_656
O29 Cu1 N1 90.3(3) . .
N23 Cu1 N1 93.6(4) 2_656 .
O29 Cu1 O27 87.5(3) . .
N23 Cu1 O27 88.7(3) 2_656 .
N1 Cu1 O27 177.4(3) . .
O29 Cu1 O28 90.2(3) . .
N23 Cu1 O28 95.7(3) 2_656 .
N1 Cu1 O28 89.1(3) . .
O27 Cu1 O28 89.6(3) . .
O32 S1 O31 111.7(5) . .
O32 S1 O33 109.1(5) . .
O31 S1 O33 110.6(4) . .
O32 S1 O30 107.6(7) . .
O31 S1 O30 109.3(5) . .
O33 S1 O30 108.5(5) . .
C2 N1 C6 118.1(9) . .
C2 N1 Cu1 123.5(7) . .
C6 N1 Cu1 117.8(7) . .
N1 C2 C3 122.7(9) . .
N1 C2 H2 118.7 . .
C3 C2 H2 118.7 . .
C2 C3 C4 118.7(9) . .
C2 C3 N7 124.5(9) . .
C4 C3 N7 116.7(9) . .
C3 C4 C5 118.5(10) . .
C3 C4 H4 120.8 . .
C5 C4 H4 120.8 . .
C6 C5 C4 120.4(10) . .
C6 C5 H5 119.8 . .
C4 C5 H5 119.8 . .
C5 C6 N1 121.4(10) . .
C5 C6 H6 119.3 . .
N1 C6 H6 119.3 . .
C8 N7 C3 128.5(9) . .
C8 N7 H7 115.7 . .
C3 N7 H7 115.7 . .
O9 C8 N7 123.5(9) . .
O9 C8 N10 124.5(9) . .
N7 C8 N10 112.0(8) . .
C8 N10 C11 128.2(8) . .
C8 N10 H10 115.9 . .
C11 N10 H10 115.9 . .
C16 C11 C12 119.0(10) . .
C16 C11 N10 117.4(9) . .
C12 C11 N10 123.6(9) . .
C13 C12 C11 119.5(11) . .
C13 C12 H12 120.3 . .
C11 C12 H12 120.3 . .
C12 C13 C14 121.8(12) . .
C12 C13 H13 119.1 . .
C14 C13 H13 119.1 . .
C15 C14 C13 117.7(11) . .
C15 C14 H14 121.1 . .
C13 C14 H14 121.1 . .
C16 C15 C14 120.8(10) . .
C16 C15 N17 116.0(9) . .
C14 C15 N17 123.2(9) . .
C15 C16 C11 121.1(10) . .
C15 C16 H16 119.4 . .
C11 C16 H16 119.4 . .
C18 N17 C15 126.5(8) . .
C18 N17 H17 116.7 . .
C15 N17 H17 116.7 . .
O19 C18 N20 123.4(9) . .
O19 C18 N17 123.9(9) . .
N20 C18 N17 112.6(9) . .
C18 N20 C21 129.6(9) . .
C18 N20 H20 115.2 . .
C21 N20 H20 115.2 . .
C22 C21 C26 118.9(9) . .
C22 C21 N20 122.5(9) . .
C26 C21 N20 118.6(9) . .
C21 C22 N23 120.9(8) . .
C21 C22 H22 119.6 . .
N23 C22 H22 119.6 . .
C24 N23 C22 118.4(8) . .
C24 N23 Cu1 120.8(7) . 2_646
C22 N23 Cu1 120.7(6) . 2_646
N23 C24 C25 122.7(10) . .
N23 C24 H24 118.6 . .
C25 C24 H24 118.6 . .
C26 C25 C24 118.4(10) . .
C26 C25 H25 120.8 . .
C24 C25 H25 120.8 . .
C25 C26 C21 120.8(10) . .
C25 C26 H26 119.6 . .
C21 C26 H26 119.6 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Cu1 O29 1.987(6) .
Cu1 N23 1.995(8) 2_656
Cu1 N1 2.037(8) .
Cu1 O27 2.039(7) .
Cu1 O28 2.278(7) .
S1 O32 1.427(9) .
S1 O31 1.455(7) .
S1 O33 1.464(8) .
S1 O30 1.464(9) .
N1 C2 1.333(12) .
N1 C6 1.383(13) .
C2 C3 1.380(14) .
C2 H2 0.9300 .
C3 C4 1.387(15) .
C3 N7 1.420(13) .
C4 C5 1.389(15) .
C4 H4 0.9300 .
C5 C6 1.342(15) .
C5 H5 0.9300 .
C6 H6 0.9300 .
N7 C8 1.342(13) .
N7 H7 0.8600 .
C8 O9 1.222(12) .
C8 N10 1.368(13) .
N10 C11 1.438(12) .
N10 H10 0.8600 .
C11 C16 1.374(14) .
C11 C12 1.378(15) .
C12 C13 1.343(18) .
C12 H12 0.9300 .
C13 C14 1.400(18) .
C13 H13 0.9300 .
C14 C15 1.360(16) .
C14 H14 0.9300 .
C15 C16 1.351(14) .
C15 N17 1.424(13) .
C16 H16 0.9300 .
N17 C18 1.381(12) .
N17 H17 0.8600 .
C18 O19 1.219(12) .
C18 N20 1.332(13) .
N20 C21 1.402(12) .
N20 H20 0.8600 .
C21 C22 1.365(13) .
C21 C26 1.393(13) .
C22 N23 1.377(12) .
C22 H22 0.9300 .
N23 C24 1.334(14) .
N23 Cu1 1.995(8) 2_646
C24 C25 1.385(15) .
C24 H24 0.9300 .
C25 C26 1.340(14) .
C25 H25 0.9300 .
C26 H26 0.9300 .
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N7 H7 O30 0.86 2.05 2.885(12) 163.9 2_745
N10 H10 O33 0.86 2.05 2.896(10) 166.1 2_745
N17 H17 O32 0.86 2.17 2.983(12) 158.0 2_645
N20 H20 O32 0.86 2.28 3.091(13) 157.1 2_645
N20 H20 O33 0.86 2.64 3.113(12) 116.1 2_645
