#------------------------------------------------------------------------------
#$Date: 2017-04-05 12:34:25 +0300 (Wed, 05 Apr 2017) $
#$Revision: 195030 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/22/77/7227764.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_7227764
loop_
_publ_author_name
'Huang, Guo-Zhen'
'Zou, Xin'
'Zhu, Zhi-Biao'
'Deng, Zhao-Peng'
'Huo, Li-Hua'
'Gao, Shan'
_publ_section_title
;
 Effect of ligand configurations, secondary Pb--O interactions and
 auxiliary ligands on Pb(ii)--mono/disulfonate complexes: syntheses,
 structures, and luminescence properties
;
_journal_issue                   13
_journal_name_full               CrystEngComm
_journal_page_first              1778
_journal_paper_doi               10.1039/C7CE00071E
_journal_volume                  19
_journal_year                    2017
_chemical_formula_moiety         'C16 H13 Cl N2 O8 Pb S2, H2 O'
_chemical_formula_sum            'C16 H15 Cl N2 O9 Pb S2'
_chemical_formula_weight         686.06
_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
_audit_update_record
;
2014-06-26 deposited with the CCDC.
2017-02-27 downloaded from the CCDC.
;
_cell_angle_alpha                99.041(11)
_cell_angle_beta                 102.300(9)
_cell_angle_gamma                108.323(12)
_cell_formula_units_Z            2
_cell_length_a                   8.5537(10)
_cell_length_b                   9.2608(15)
_cell_length_c                   13.8202(14)
_cell_measurement_reflns_used    1841
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      27.54
_cell_measurement_theta_min      3.16
_cell_volume                     985.3(2)
_computing_cell_refinement
;
CrysAlis Pro (Agilent, 2013)
;
_computing_data_collection
;
CrysAlis Pro (Agilent, 2013)
;
_computing_data_reduction
;
CrysAlis Pro (Agilent, 2013)
;
_computing_molecular_graphics    '(K. Brandenburg, Diamond 3.1, 2009)'
_computing_publication_material  '(K. Brandenburg, Diamond 3.1, 2009)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      295(2)
_diffrn_detector_area_resol_mean 16.1954
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0448
_diffrn_reflns_av_sigmaI/netI    0.0875
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            6434
_diffrn_reflns_theta_full        27.56
_diffrn_reflns_theta_max         27.56
_diffrn_reflns_theta_min         3.16
_exptl_absorpt_coefficient_mu    8.965
_exptl_absorpt_correction_T_max  0.2952
_exptl_absorpt_correction_T_min  0.2547
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
CrysAlis Pro (Agilent, 2013)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm. 
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.312
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             656
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.18
_refine_diff_density_max         1.794
_refine_diff_density_min         -1.707
_refine_diff_density_rms         0.217
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     280
_refine_ls_number_reflns         4493
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0702
_refine_ls_R_factor_gt           0.0555
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0514P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1197
_refine_ls_wR_factor_ref         0.1302
_reflns_number_gt                3670
_reflns_number_total             4493
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c7ce00071e2.cif
_cod_data_source_block           complex8
_cod_depositor_comments
'Adding full bibliography for 7227757--7227764.cif.'
_cod_database_code               7227764
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
Pb1 Pb 0.82952(4) -0.09824(4) 0.57172(3) 0.03659(14) Uani 1 1 d .
Cl1 Cl 0.4048(3) 0.1274(4) 0.09747(18) 0.0515(7) Uani 1 1 d .
S1 S 0.6905(3) 0.2219(3) 0.50067(17) 0.0384(6) Uani 1 1 d .
S2 S 0.8195(3) -0.1868(3) 0.21120(18) 0.0376(5) Uani 1 1 d .
O1 O 0.8494(10) 0.3568(10) 0.5253(6) 0.061(2) Uani 1 1 d .
O1W O 0.8153(11) -0.3524(10) 0.4520(7) 0.072(3) Uani 1 1 d .
H1W1 H 0.7508 -0.3830 0.3911 0.086 Uiso 1 1 d R
H1W2 H 0.8751 -0.4046 0.4739 0.086 Uiso 1 1 d R
O2W O 0.4570(15) -0.5012(13) 0.3448(9) 0.101(4) Uani 1 1 d .
H2W1 H 0.3620 -0.5730 0.3387 0.122 Uiso 1 1 d R
H2W2 H 0.4411 -0.4528 0.2984 0.122 Uiso 1 1 d R
O2 O 0.5409(9) 0.2688(10) 0.4967(5) 0.0514(19) Uani 1 1 d .
O3 O 0.6993(9) 0.1171(9) 0.5674(5) 0.0497(19) Uani 1 1 d .
O4 O 0.7413(10) -0.3265(9) 0.2421(6) 0.0543(19) Uani 1 1 d .
O5 O 0.7870(10) -0.2109(10) 0.1012(5) 0.056(2) Uani 1 1 d .
O6 O 1.0040(8) -0.1115(9) 0.2634(5) 0.0469(18) Uani 1 1 d .
O7 O 0.8706(7) 0.0036(8) 0.4272(4) 0.0329(14) Uani 1 1 d .
H7O H 0.8546 -0.0866 0.3923 0.049 Uiso 1 1 d R
N1 N 0.9463(11) -0.2512(11) 0.7253(7) 0.048(2) Uani 1 1 d .
N2 N 1.3317(11) -0.4001(11) 1.1887(7) 0.051(2) Uani 1 1 d .
C1 C 0.6568(11) 0.1169(11) 0.3741(6) 0.0297(19) Uani 1 1 d .
C2 C 0.7538(11) 0.0227(11) 0.3526(7) 0.033(2) Uani 1 1 d .
C3 C 0.7209(10) -0.0519(11) 0.2497(6) 0.0299(19) Uani 1 1 d .
C4 C 0.6109(11) -0.0217(12) 0.1701(7) 0.035(2) Uani 1 1 d .
H4 H 0.5931 -0.0693 0.1022 0.042 Uiso 1 1 calc R
C5 C 0.5304(11) 0.0812(12) 0.1961(7) 0.033(2) Uani 1 1 d .
C6 C 0.5514(11) 0.1503(12) 0.2966(7) 0.036(2) Uani 1 1 d .
H6 H 0.4955 0.2185 0.3121 0.043 Uiso 1 1 calc R
C7 C 0.9301(13) -0.1888(15) 0.8142(9) 0.052(3) Uani 1 1 d .
H7 H 0.8689 -0.1218 0.8149 0.063 Uiso 1 1 calc R
C8 C 1.0010(13) -0.2186(13) 0.9078(9) 0.048(3) Uani 1 1 d .
H8 H 0.9814 -0.1762 0.9677 0.057 Uiso 1 1 calc R
C9 C 1.1003(12) -0.3120(12) 0.9093(7) 0.039(2) Uani 1 1 d .
C10 C 1.1162(13) -0.3760(13) 0.8160(7) 0.044(2) Uani 1 1 d .
H10 H 1.1789 -0.4416 0.8128 0.053 Uiso 1 1 calc R
C11 C 1.0398(14) -0.3432(13) 0.7277(8) 0.047(3) Uani 1 1 d .
H11 H 1.0542 -0.3874 0.6665 0.056 Uiso 1 1 calc R
C12 C 1.2423(13) -0.3030(13) 1.1892(8) 0.046(2) Uani 1 1 d .
H12 H 1.2319 -0.2554 1.2508 0.056 Uiso 1 1 calc R
C13 C 1.1668(13) -0.2738(13) 1.1005(7) 0.046(2) Uani 1 1 d .
H13 H 1.1037 -0.2084 1.1026 0.055 Uiso 1 1 calc R
C14 C 1.1825(11) -0.3400(11) 1.0069(7) 0.034(2) Uani 1 1 d .
C15 C 1.2768(13) -0.4391(13) 1.0079(8) 0.046(3) Uani 1 1 d .
H15 H 1.2917 -0.4852 0.9474 0.055 Uiso 1 1 calc R
C16 C 1.3475(13) -0.4682(13) 1.0984(8) 0.047(3) Uani 1 1 d .
H16 H 1.4076 -0.5361 1.0979 0.056 Uiso 1 1 calc R
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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pb Pb -3.3944 10.1111 '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
O7 Pb1 O7 67.7(2) . 2_756
O7 Pb1 O6 110.7(2) . 2_756
O7 Pb1 O6 72.5(2) 2_756 2_756
O7 Pb1 O3 72.1(2) . .
O7 Pb1 O3 112.3(2) 2_756 .
O6 Pb1 O3 74.1(2) 2_756 .
O7 Pb1 O1W 81.5(2) . .
O7 Pb1 O1W 83.9(2) 2_756 .
O6 Pb1 O1W 145.6(2) 2_756 .
O3 Pb1 O1W 139.5(3) . .
O3 S1 O1 112.7(5) . .
O3 S1 O2 111.8(4) . .
O1 S1 O2 112.0(5) . .
O3 S1 C1 108.1(4) . .
O1 S1 C1 106.8(4) . .
O2 S1 C1 105.1(4) . .
O4 S2 O5 113.2(5) . .
O4 S2 O6 112.4(4) . .
O5 S2 O6 111.2(4) . .
O4 S2 C3 106.5(4) . .
O5 S2 C3 106.3(4) . .
O6 S2 C3 106.8(4) . .
Pb1 O1W H1W1 120.0 . .
Pb1 O1W H1W2 120.0 . .
H1W1 O1W H1W2 120.0 . .
H2W1 O2W H2W2 107.9 . .
S1 O3 Pb1 133.0(4) . .
S2 O6 Pb1 132.2(4) . 2_756
C2 O7 Pb1 128.7(5) . .
C2 O7 Pb1 118.9(5) . 2_756
Pb1 O7 Pb1 112.3(2) . 2_756
C2 O7 H7O 91.2 . .
Pb1 O7 H7O 91.3 . .
Pb1 O7 H7O 91.3 2_756 .
C7 N1 C11 116.5(9) . .
C12 N2 C16 119.1(9) . .
C6 C1 C2 121.5(8) . .
C6 C1 S1 116.6(7) . .
C2 C1 S1 121.2(6) . .
O7 C2 C3 121.3(8) . .
O7 C2 C1 121.9(8) . .
C3 C2 C1 116.8(7) . .
C2 C3 C4 121.9(8) . .
C2 C3 S2 122.2(6) . .
C4 C3 S2 115.9(7) . .
C5 C4 C3 118.0(8) . .
C5 C4 H4 121.0 . .
C3 C4 H4 121.0 . .
C6 C5 C4 122.0(8) . .
C6 C5 Cl1 120.1(7) . .
C4 C5 Cl1 117.9(7) . .
C5 C6 C1 119.3(8) . .
C5 C6 H6 120.3 . .
C1 C6 H6 120.3 . .
N1 C7 C8 123.6(10) . .
N1 C7 H7 118.2 . .
C8 C7 H7 118.2 . .
C9 C8 C7 119.2(10) . .
C9 C8 H8 120.4 . .
C7 C8 H8 120.4 . .
C10 C9 C8 116.4(9) . .
C10 C9 C14 123.0(9) . .
C8 C9 C14 120.5(9) . .
C11 C10 C9 120.6(10) . .
C11 C10 H10 119.7 . .
C9 C10 H10 119.7 . .
N1 C11 C10 123.6(10) . .
N1 C11 H11 118.2 . .
C10 C11 H11 118.2 . .
N2 C12 C13 120.9(10) . .
N2 C12 H12 119.5 . .
C13 C12 H12 119.5 . .
C12 C13 C14 121.3(10) . .
C12 C13 H13 119.3 . .
C14 C13 H13 119.3 . .
C13 C14 C15 117.0(9) . .
C13 C14 C9 122.5(9) . .
C15 C14 C9 120.5(8) . .
C16 C15 C14 119.9(10) . .
C16 C15 H15 120.0 . .
C14 C15 H15 120.0 . .
N2 C16 C15 121.7(10) . .
N2 C16 H16 119.1 . .
C15 C16 H16 119.1 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Pb1 O7 2.385(6) .
Pb1 O7 2.432(6) 2_756
Pb1 O6 2.546(7) 2_756
Pb1 O3 2.574(7) .
Pb1 O1W 2.608(8) .
Cl1 C5 1.744(9) .
S1 O3 1.447(7) .
S1 O1 1.458(8) .
S1 O2 1.469(6) .
S1 C1 1.779(9) .
S2 O4 1.434(8) .
S2 O5 1.454(7) .
S2 O6 1.470(7) .
S2 C3 1.789(8) .
O1W H1W1 0.8500 .
O1W H1W2 0.8499 .
O2W H2W1 0.8499 .
O2W H2W2 0.8500 .
O6 Pb1 2.546(7) 2_756
O7 C2 1.349(10) .
O7 Pb1 2.432(6) 2_756
O7 H7O 0.8500 .
N1 C7 1.327(14) .
N1 C11 1.339(13) .
N2 C12 1.351(14) .
N2 C16 1.361(13) .
C1 C6 1.387(11) .
C1 C2 1.420(12) .
C2 C3 1.406(12) .
C3 C4 1.412(11) .
C4 C5 1.387(12) .
C4 H4 0.9300 .
C5 C6 1.382(12) .
C6 H6 0.9300 .
C7 C8 1.415(14) .
C7 H7 0.9300 .
C8 C9 1.389(13) .
C8 H8 0.9300 .
C9 C10 1.385(14) .
C9 C14 1.484(13) .
C10 C11 1.383(14) .
C10 H10 0.9300 .
C11 H11 0.9300 .
C12 C13 1.368(14) .
C12 H12 0.9300 .
C13 C14 1.394(13) .
C13 H13 0.9300 .
C14 C15 1.399(13) .
C15 C16 1.373(13) .
C15 H15 0.9300 .
C16 H16 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
O1W H1W1 O4 0.85 2.19 2.899(12) 140.3 .
O1W H1W1 O2W 0.85 2.30 2.873(14) 125.0 .
O1W H1W2 O1 0.85 2.25 2.831(11) 125.3 2_756
O1W H1W2 O1 0.85 2.39 3.097(13) 141.6 1_545
O2W H2W2 N2 0.85 1.82 2.638(15) 159.8 1_454
O7 H7O O6 0.85 2.43 2.944(9) 120.0 .
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
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_4
O1 S1 O3 Pb1 -80.0(7) . .
O2 S1 O3 Pb1 152.9(5) . .
C1 S1 O3 Pb1 37.7(7) . .
O7 Pb1 O3 S1 -2.2(6) . .
O7 Pb1 O3 S1 53.5(7) 2_756 .
O6 Pb1 O3 S1 116.4(6) 2_756 .
O1W Pb1 O3 S1 -54.2(8) . .
O4 S2 O6 Pb1 -91.0(6) . 2_756
O5 S2 O6 Pb1 141.0(5) . 2_756
C3 S2 O6 Pb1 25.5(7) . 2_756
O7 Pb1 O7 C2 -175.5(9) 2_756 .
O6 Pb1 O7 C2 -115.7(7) 2_756 .
O3 Pb1 O7 C2 -51.2(7) . .
O1W Pb1 O7 C2 97.6(7) . .
O7 Pb1 O7 Pb1 0.0 2_756 2_756
O6 Pb1 O7 Pb1 59.8(3) 2_756 2_756
O3 Pb1 O7 Pb1 124.2(3) . 2_756
O1W Pb1 O7 Pb1 -86.9(3) . 2_756
O3 S1 C1 C6 143.6(7) . .
O1 S1 C1 C6 -95.0(8) . .
O2 S1 C1 C6 24.1(9) . .
O3 S1 C1 C2 -46.0(9) . .
O1 S1 C1 C2 75.5(9) . .
O2 S1 C1 C2 -165.4(8) . .
Pb1 O7 C2 C3 -120.7(8) . .
Pb1 O7 C2 C3 64.1(10) 2_756 .
Pb1 O7 C2 C1 58.5(12) . .
Pb1 O7 C2 C1 -116.8(8) 2_756 .
C6 C1 C2 O7 172.6(9) . .
S1 C1 C2 O7 2.6(13) . .
C6 C1 C2 C3 -8.2(14) . .
S1 C1 C2 C3 -178.2(7) . .
O7 C2 C3 C4 -174.0(9) . .
C1 C2 C3 C4 6.8(14) . .
O7 C2 C3 S2 4.4(13) . .
C1 C2 C3 S2 -174.8(7) . .
O4 S2 C3 C2 71.8(9) . .
O5 S2 C3 C2 -167.3(8) . .
O6 S2 C3 C2 -48.5(9) . .
O4 S2 C3 C4 -109.7(8) . .
O5 S2 C3 C4 11.2(9) . .
O6 S2 C3 C4 130.0(7) . .
C2 C3 C4 C5 -2.0(14) . .
S2 C3 C4 C5 179.5(7) . .
C3 C4 C5 C6 -1.7(15) . .
C3 C4 C5 Cl1 176.2(7) . .
C4 C5 C6 C1 0.3(15) . .
Cl1 C5 C6 C1 -177.6(7) . .
C2 C1 C6 C5 4.8(15) . .
S1 C1 C6 C5 175.2(7) . .
C11 N1 C7 C8 -2.0(16) . .
N1 C7 C8 C9 3.2(17) . .
C7 C8 C9 C10 -2.9(16) . .
C7 C8 C9 C14 177.4(10) . .
C8 C9 C10 C11 1.7(16) . .
C14 C9 C10 C11 -178.6(10) . .
C7 N1 C11 C10 0.7(16) . .
C9 C10 C11 N1 -0.6(17) . .
C16 N2 C12 C13 0.6(16) . .
N2 C12 C13 C14 -1.5(17) . .
C12 C13 C14 C15 0.8(15) . .
C12 C13 C14 C9 179.2(10) . .
C10 C9 C14 C13 179.4(10) . .
C8 C9 C14 C13 -0.9(15) . .
C10 C9 C14 C15 -2.2(15) . .
C8 C9 C14 C15 177.4(10) . .
C13 C14 C15 C16 0.6(15) . .
C9 C14 C15 C16 -177.8(10) . .
C12 N2 C16 C15 0.9(17) . .
C14 C15 C16 N2 -1.5(17) . .
