#------------------------------------------------------------------------------
#$Date: 2016-03-25 21:51:44 +0100 (vie 25 de mar de 2016) $
#$Revision: 180017 $
#$URL: svn://www.crystallography.net/cod/cif/7/03/11/7031114.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_7031114
loop_
_publ_author_name
'Zhang, Kou-Lin'
'Zhong, Zhao-Yin'
'Zhang, Lei'
'Jing, Chu-Yue'
'Daniels, Luke M.'
'Walton, Richard I.'
_publ_section_title
;
 Synthesis, characterization and properties of a family of
 lead(ii)-organic frameworks based on a multi-functional ligand
 2-amino-4-sulfobenzoic acid exhibiting auxiliary ligand-dependent
 dehydration-rehydration behaviours.
;
_journal_issue                   30
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              11597
_journal_page_last               11610
_journal_paper_doi               10.1039/c4dt00659c
_journal_volume                  43
_journal_year                    2014
_chemical_formula_sum            'C14 H16 N2 O11 S2'
_chemical_formula_weight         452.41
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_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                93.554(5)
_cell_angle_beta                 97.654(6)
_cell_angle_gamma                102.178(6)
_cell_formula_units_Z            1
_cell_length_a                   6.2881(12)
_cell_length_b                   8.0961(14)
_cell_length_c                   8.6404(14)
_cell_measurement_reflns_used    3553
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      27.0839
_cell_measurement_theta_min      2.5849
_cell_volume                     424.30(13)
_computing_cell_refinement       'SAINT (Bruker, 2005)'
_computing_data_collection       'APEX2 (Bruker, 2005)'
_computing_data_reduction        'SAINT (Bruker, 2005)'
_computing_molecular_graphics    'Diamond (CRYSTAL IMPACT, 2001)'
_computing_publication_material  'publCIF (Westrip, 2010)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      296(2)
_diffrn_detector_area_resol_mean 8.3
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEXII area-detector'
_diffrn_measurement_method       'φ and ω'
_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  0.0445
_diffrn_reflns_av_sigmaI/netI    0.0381
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            8567
_diffrn_reflns_theta_full        27.56
_diffrn_reflns_theta_max         27.56
_diffrn_reflns_theta_min         2.58
_exptl_absorpt_coefficient_mu    0.385
_exptl_absorpt_correction_T_max  0.912
_exptl_absorpt_correction_T_min  0.884
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.771
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             234
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.24
_refine_diff_density_max         0.351
_refine_diff_density_min         -0.327
_refine_diff_density_rms         0.067
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     135
_refine_ls_number_reflns         1955
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.061
_refine_ls_R_factor_all          0.0529
_refine_ls_R_factor_gt           0.0387
_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)+(0.0456P)²+0.2654P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0934
_refine_ls_wR_factor_ref         0.1002
_reflns_number_gt                1598
_reflns_number_total             1955
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4dt00659c2.cif
_cod_data_source_block           zl05
_cod_depositor_comments
'Adding full bibliography for 7031110--7031114.cif.'
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7031114
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
C1 C 0.2192(3) 0.2832(2) 0.1568(2) 0.0232(4) Uani 1 1 d .
C2 C 0.0001(3) 0.2108(2) 0.1678(2) 0.0216(4) Uani 1 1 d .
C3 C -0.1588(3) 0.1726(2) 0.0358(2) 0.0224(4) Uani 1 1 d .
H3 H -0.3040 0.1241 0.0446 0.027 Uiso 1 1 calc R
C4 C -0.0995(3) 0.2072(2) -0.1091(2) 0.0223(4) Uani 1 1 d .
C5 C 0.1169(4) 0.2783(3) -0.1237(2) 0.0337(5) Uani 1 1 d .
H5 H 0.1561 0.3012 -0.2215 0.040 Uiso 1 1 calc R
C6 C 0.2737(4) 0.3146(3) 0.0095(3) 0.0315(5) Uani 1 1 d .
H6 H 0.4192 0.3612 -0.0001 0.038 Uiso 1 1 calc R
C7 C 0.4048(3) 0.3253(2) 0.2921(2) 0.0254(4) Uani 1 1 d .
N1 N -0.0697(3) 0.1665(3) 0.31747(19) 0.0304(4) Uani 1 1 d .
H1A H -0.2111 0.1138 0.3014 0.046 Uiso 1 1 calc R
H1B H -0.0510 0.2606 0.3814 0.046 Uiso 1 1 calc R
H1C H 0.0106 0.0983 0.3607 0.046 Uiso 1 1 calc R
O1 O 0.3405(2) 0.3080(2) 0.43029(16) 0.0311(4) Uani 1 1 d .
H1 H 0.4481 0.3149 0.4974 0.047 Uiso 1 1 calc R
O2 O 0.5939(2) 0.3719(2) 0.27298(19) 0.0379(4) Uani 1 1 d .
O3 O -0.4841(3) 0.0362(2) -0.23777(17) 0.0378(4) Uani 1 1 d .
O4 O -0.3511(3) 0.3122(2) -0.32488(18) 0.0392(4) Uani 1 1 d .
O5 O -0.1905(3) 0.0788(2) -0.39607(17) 0.0350(4) Uani 1 1 d .
O1W O 0.0000 0.5000 0.5000 0.0508(7) Uani 1 2 d SD
H1WA H 0.0469 0.5383 0.4171 0.061 Uiso 0.50 1 d PRD
H1WB H 0.1155 0.5003 0.5662 0.061 Uiso 0.50 1 d PRD
S1 S -0.30013(8) 0.15279(6) -0.28101(5) 0.02307(16) Uani 1 1 d .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
C1 0.0200(10) 0.0245(10) 0.0231(10) 0.0000(8) -0.0018(8) 0.0044(8)
C2 0.0206(10) 0.0272(10) 0.0179(9) 0.0036(7) 0.0032(7) 0.0068(8)
C3 0.0165(9) 0.0293(10) 0.0208(9) 0.0019(8) 0.0017(7) 0.0046(8)
C4 0.0221(10) 0.0265(10) 0.0167(9) 0.0034(7) -0.0008(7) 0.0039(8)
C5 0.0294(12) 0.0454(13) 0.0210(10) 0.0077(9) 0.0044(9) -0.0053(10)
C6 0.0219(10) 0.0382(12) 0.0286(11) 0.0055(9) 0.0032(8) -0.0065(9)
C7 0.0228(11) 0.0220(9) 0.0288(11) -0.0011(8) -0.0033(8) 0.0046(8)
N1 0.0208(9) 0.0510(11) 0.0181(8) 0.0044(8) 0.0019(7) 0.0054(8)
O1 0.0252(8) 0.0418(9) 0.0227(7) 0.0019(6) -0.0074(6) 0.0064(7)
O2 0.0193(8) 0.0506(10) 0.0387(9) -0.0021(7) -0.0027(7) 0.0026(7)
O3 0.0269(8) 0.0517(10) 0.0255(8) 0.0056(7) -0.0013(6) -0.0091(7)
O4 0.0495(10) 0.0322(8) 0.0326(9) 0.0040(7) -0.0130(7) 0.0136(7)
O5 0.0411(10) 0.0439(9) 0.0204(7) 0.0001(6) 0.0040(6) 0.0119(7)
O1W 0.0287(13) 0.0531(15) 0.0675(18) -0.0033(13) 0.0056(12) 0.0055(11)
S1 0.0237(3) 0.0275(3) 0.0156(2) 0.00364(18) -0.00174(18) 0.00289(19)
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'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
C6 C1 C2 118.08(17)
C6 C1 C7 116.64(18)
C2 C1 C7 125.24(18)
C3 C2 C1 121.12(18)
C3 C2 N1 117.20(17)
C1 C2 N1 121.64(17)
C4 C3 C2 119.37(18)
C4 C3 H3 120.3
C2 C3 H3 120.3
C3 C4 C5 120.80(18)
C3 C4 S1 119.98(15)
C5 C4 S1 119.17(15)
C6 C5 C4 118.97(19)
C6 C5 H5 120.5
C4 C5 H5 120.5
C5 C6 C1 121.65(19)
C5 C6 H6 119.2
C1 C6 H6 119.2
O2 C7 O1 124.13(18)
O2 C7 C1 121.99(19)
O1 C7 C1 113.88(17)
C2 N1 H1A 109.5
C2 N1 H1B 109.5
H1A N1 H1B 109.5
C2 N1 H1C 109.5
H1A N1 H1C 109.5
H1B N1 H1C 109.5
C7 O1 H1 109.5
H1WA O1W H1WB 106.2
O3 S1 O5 113.87(10)
O3 S1 O4 113.46(11)
O5 S1 O4 111.92(10)
O3 S1 C4 106.28(9)
O5 S1 C4 104.84(9)
O4 S1 C4 105.54(9)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
C1 C6 1.386(3)
C1 C2 1.397(3)
C1 C7 1.505(3)
C2 C3 1.384(3)
C2 N1 1.461(2)
C3 C4 1.382(3)
C3 H3 0.9300
C4 C5 1.387(3)
C4 S1 1.7824(19)
C5 C6 1.384(3)
C5 H5 0.9300
C6 H6 0.9300
C7 O2 1.206(2)
C7 O1 1.317(3)
N1 H1A 0.8900
N1 H1B 0.8900
N1 H1C 0.8900
O1 H1 0.8200
O3 S1 1.4374(16)
O4 S1 1.4545(16)
O5 S1 1.4511(16)
O1W H1WA 0.8611
O1W H1WB 0.8622
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
C6 C1 C2 C3 -0.5(3)
C7 C1 C2 C3 -178.38(18)
C6 C1 C2 N1 177.25(19)
C7 C1 C2 N1 -0.6(3)
C1 C2 C3 C4 -0.2(3)
N1 C2 C3 C4 -178.04(17)
C2 C3 C4 C5 0.5(3)
C2 C3 C4 S1 178.05(15)
C3 C4 C5 C6 -0.1(3)
S1 C4 C5 C6 -177.67(17)
C4 C5 C6 C1 -0.6(3)
C2 C1 C6 C5 0.9(3)
C7 C1 C6 C5 179.0(2)
C6 C1 C7 O2 -5.4(3)
C2 C1 C7 O2 172.5(2)
C6 C1 C7 O1 173.93(18)
C2 C1 C7 O1 -8.2(3)
C3 C4 S1 O3 -15.7(2)
C5 C4 S1 O3 161.94(17)
C3 C4 S1 O5 -136.56(17)
C5 C4 S1 O5 41.04(19)
C3 C4 S1 O4 105.11(18)
C5 C4 S1 O4 -77.29(19)
