#------------------------------------------------------------------------------
#$Date: 2018-08-29 03:11:30 +0300 (Wed, 29 Aug 2018) $
#$Revision: 210210 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/30/10/4301062.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_4301062
loop_
_publ_author_name
'Kavallieratos, Konstantinos'
'Rosenberg, Jay M.'
'Bryan, Jeffrey C.'
_publ_section_title
;
 Pb(II) Coordination and Synergistic Ion-Exchange Extraction by Combinations
 of Sulfonamide Chelates and 2,2'-Bipyridine
;
_journal_coden_ASTM              INOCAJ
_journal_issue                   8
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2573
_journal_page_last               2575
_journal_paper_doi               10.1021/ic050047r
_journal_volume                  44
_journal_year                    2005
_chemical_formula_moiety         'C18 H14 N2 O4 Pb S2'
_chemical_formula_sum            'C18 H14 N2 O4 Pb S2'
_chemical_formula_weight         593.6
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 99.828(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.8201(15)
_cell_length_b                   19.358(3)
_cell_length_c                   9.8553(12)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      14.7
_cell_measurement_theta_min      10.0
_cell_volume                     1846.0(5)
_computing_cell_refinement       'CAD4/PC (Nonius, 1996)'
_computing_data_collection       'CAD4/PC (Nonius, 1996)'
_computing_data_reduction        'XCAD4 (Harms, 1995)'
_computing_molecular_graphics    'SHELXTL (Bruker, 1997)'
_computing_publication_material  'SHELXTL (Bruker, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.98
_diffrn_measured_fraction_theta_max 0.98
_diffrn_measurement_device_type  'Enraf-Nonius CAD4'
_diffrn_measurement_method       Omega-scans
_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  0.036
_diffrn_reflns_av_sigmaI/netI    0.039
_diffrn_reflns_limit_h_max       0
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            7764
_diffrn_reflns_theta_full        27.0
_diffrn_reflns_theta_max         27.0
_diffrn_reflns_theta_min         2.3
_diffrn_standards_decay_%        -2
_diffrn_standards_interval_time  120
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    9.393
_exptl_absorpt_correction_T_max  0.3149
_exptl_absorpt_correction_T_min  0.1170
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'XPREP (Bruker, 1997)'
_exptl_crystal_colour            'very pale yellow'
_exptl_crystal_density_diffrn    2.14
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    .
_exptl_crystal_description       'hexagonal plate'
_exptl_crystal_F_000             1128
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.16
_refine_diff_density_max         1.6
_refine_diff_density_min         -2.1
_refine_diff_density_rms         0.19
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.04
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     244
_refine_ls_number_reflns         3935
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.04
_refine_ls_R_factor_all          0.040
_refine_ls_R_factor_gt           0.028
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0469P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.071
_refine_ls_wR_factor_ref         0.075
_reflns_number_gt                3322
_reflns_number_total             3935
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic050047rsi20050112_101605.cif
_cod_data_source_block           k2pb
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_database_code               4301062
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Pb Pb 0.907428(15) 0.460132(9) 0.727297(16) 0.01024(7) Uani 1 1 d . . .
S1 S 0.88336(12) 0.58878(6) 0.92906(12) 0.0133(2) Uani 1 1 d . . .
S2 S 1.19228(11) 0.44006(6) 0.59315(11) 0.0110(2) Uani 1 1 d . . .
O1 O 0.7881(4) 0.53220(17) 0.9328(4) 0.0181(8) Uani 1 1 d . . .
O2 O 0.9660(4) 0.60796(19) 1.0610(4) 0.0203(8) Uani 1 1 d . . .
O3 O 1.1048(3) 0.37936(19) 0.5802(4) 0.0177(7) Uani 1 1 d . . .
O4 O 1.2238(4) 0.46691(18) 0.4637(4) 0.0169(7) Uani 1 1 d . . .
N1 N 0.9711(4) 0.5672(2) 0.8167(4) 0.0138(8) Uani 1 1 d . . .
N2 N 1.1204(4) 0.4942(2) 0.6761(4) 0.0120(8) Uani 1 1 d . . .
C1 C 1.0913(4) 0.6012(3) 0.7883(5) 0.0142(10) Uani 1 1 d . . .
C2 C 1.1696(5) 0.5616(2) 0.7094(5) 0.0125(9) Uani 1 1 d . . .
C3 C 1.2885(5) 0.5907(3) 0.6735(5) 0.0184(10) Uani 1 1 d . . .
H3 H 1.3424 0.5650 0.6198 0.022 Uiso 1 1 calc R . .
C4 C 1.3281(5) 0.6573(3) 0.7164(6) 0.0247(12) Uani 1 1 d . . .
H4 H 1.4098 0.6767 0.6927 0.030 Uiso 1 1 calc R . .
C5 C 1.2498(5) 0.6955(3) 0.7930(6) 0.0220(11) Uani 1 1 d . . .
H5 H 1.2784 0.7408 0.8221 0.026 Uiso 1 1 calc R . .
C6 C 1.1300(5) 0.6684(3) 0.8279(5) 0.0186(10) Uani 1 1 d . . .
H6 H 1.0748 0.6953 0.8782 0.022 Uiso 1 1 calc R . .
C11 C 0.7845(5) 0.6630(3) 0.8725(5) 0.0147(9) Uani 1 1 d . . .
C12 C 0.7253(5) 0.6997(3) 0.9682(5) 0.0171(10) Uani 1 1 d . . .
H12 H 0.7469 0.6886 1.0633 0.021 Uiso 1 1 calc R . .
C13 C 0.6340(5) 0.7532(3) 0.9230(6) 0.0205(11) Uani 1 1 d . . .
H13 H 0.5915 0.7784 0.9871 0.025 Uiso 1 1 calc R . .
C14 C 0.6050(5) 0.7694(3) 0.7834(6) 0.0213(12) Uani 1 1 d . . .
H14 H 0.5415 0.8053 0.7521 0.026 Uiso 1 1 calc R . .
C15 C 0.6683(5) 0.7334(3) 0.6906(6) 0.0198(11) Uani 1 1 d . . .
H15 H 0.6495 0.7456 0.5959 0.024 Uiso 1 1 calc R . .
C16 C 0.7594(5) 0.6794(2) 0.7334(5) 0.0155(10) Uani 1 1 d . . .
H16 H 0.8029 0.6546 0.6694 0.019 Uiso 1 1 calc R . .
C21 C 1.3548(4) 0.4174(2) 0.6891(5) 0.0120(9) Uani 1 1 d . . .
C22 C 1.4476(5) 0.3829(3) 0.6216(5) 0.0179(10) Uani 1 1 d . . .
H22 H 1.4259 0.3748 0.5253 0.021 Uiso 1 1 calc R . .
C23 C 1.5720(5) 0.3603(3) 0.6959(6) 0.0226(11) Uani 1 1 d . . .
H23 H 1.6351 0.3354 0.6514 0.027 Uiso 1 1 calc R . .
C24 C 1.6041(5) 0.3745(3) 0.8363(6) 0.0230(11) Uani 1 1 d . . .
H24 H 1.6901 0.3595 0.8870 0.028 Uiso 1 1 calc R . .
C25 C 1.5132(5) 0.4098(3) 0.9026(5) 0.0211(11) Uani 1 1 d . . .
H25 H 1.5366 0.4190 0.9984 0.025 Uiso 1 1 calc R . .
C26 C 1.3871(5) 0.4319(3) 0.8296(5) 0.0170(10) Uani 1 1 d . . .
H26 H 1.3239 0.4566 0.8746 0.020 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'
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
_geom_angle_publ_flag
N1 Pb N2 68.40(14) . . ?
N1 Pb O4 81.49(12) . 3_766 ?
N2 Pb O4 92.47(13) . 3_766 ?
N1 Pb O2 95.05(13) . 3_767 ?
N2 Pb O2 89.62(13) . 3_767 ?
O4 Pb O2 174.97(11) 3_766 3_767 ?
O1 S1 O2 115.7(2) . . ?
O1 S1 N1 104.6(2) . . ?
O2 S1 N1 114.0(2) . . ?
O1 S1 C11 107.5(2) . . ?
O2 S1 C11 105.4(2) . . ?
N1 S1 C11 109.4(2) . . ?
O3 S2 O4 115.0(2) . . ?
O3 S2 N2 106.0(2) . . ?
O4 S2 N2 113.5(2) . . ?
O3 S2 C21 108.3(2) . . ?
O4 S2 C21 104.5(2) . . ?
N2 S2 C21 109.4(2) . . ?
S1 O2 Pb 134.7(2) . 3_767 ?
S2 O4 Pb 133.9(2) . 3_766 ?
C1 N1 S1 126.1(3) . . ?
C1 N1 Pb 121.6(3) . . ?
S1 N1 Pb 111.4(2) . . ?
C2 N2 S2 124.9(3) . . ?
C2 N2 Pb 119.8(3) . . ?
S2 N2 Pb 115.1(2) . . ?
C6 C1 C2 121.0(4) . . ?
C6 C1 N1 125.1(4) . . ?
C2 C1 N1 113.9(4) . . ?
C3 C2 N2 125.7(4) . . ?
C3 C2 C1 118.6(4) . . ?
N2 C2 C1 115.7(4) . . ?
C4 C3 C2 120.0(5) . . ?
C5 C4 C3 120.7(5) . . ?
C4 C5 C6 120.6(5) . . ?
C5 C6 C1 119.2(5) . . ?
C12 C11 C16 122.1(5) . . ?
C12 C11 S1 118.2(4) . . ?
C16 C11 S1 119.5(4) . . ?
C11 C12 C13 119.0(5) . . ?
C12 C13 C14 119.8(5) . . ?
C15 C14 C13 120.1(5) . . ?
C14 C15 C16 121.1(5) . . ?
C11 C16 C15 117.9(5) . . ?
C22 C21 C26 121.0(4) . . ?
C22 C21 S2 118.1(4) . . ?
C26 C21 S2 120.9(4) . . ?
C23 C22 C21 119.4(5) . . ?
C22 C23 C24 119.6(5) . . ?
C25 C24 C23 121.0(5) . . ?
C24 C25 C26 120.1(5) . . ?
C25 C26 C21 118.9(4) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pb N1 2.296(4) . ?
Pb N2 2.329(4) . ?
Pb O4 2.524(3) 3_766 ?
Pb O2 2.599(3) 3_767 ?
S1 O1 1.445(4) . ?
S1 O2 1.458(4) . ?
S1 N1 1.571(4) . ?
S1 C11 1.770(5) . ?
S2 O3 1.448(4) . ?
S2 O4 1.459(4) . ?
S2 N2 1.569(4) . ?
S2 C21 1.766(5) . ?
O2 Pb 2.599(3) 3_767 ?
O4 Pb 2.524(3) 3_766 ?
N1 C1 1.421(6) . ?
N2 C2 1.410(6) . ?
C1 C6 1.391(7) . ?
C1 C2 1.411(7) . ?
C2 C3 1.395(7) . ?
C3 C4 1.392(7) . ?
C4 C5 1.381(8) . ?
C5 C6 1.384(7) . ?
C11 C12 1.385(7) . ?
C11 C16 1.387(7) . ?
C12 C13 1.392(7) . ?
C13 C14 1.392(8) . ?
C14 C15 1.380(8) . ?
C15 C16 1.393(7) . ?
C21 C22 1.388(7) . ?
C21 C26 1.395(7) . ?
C22 C23 1.383(7) . ?
C23 C24 1.393(8) . ?
C24 C25 1.375(8) . ?
C25 C26 1.390(7) . ?
