#------------------------------------------------------------------------------
#$Date: 2016-03-25 23:00:38 +0200 (Fri, 25 Mar 2016) $
#$Revision: 180022 $
#$URL: svn://www.crystallography.net/cod/cif/7/03/16/7031676.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_7031676
loop_
_publ_author_name
'Imran, Muhammad'
'Mix, Andreas'
'Neumann, Beate'
'Stammler, Hans-Georg'
'Monkowius, Uwe'
'Gründlinger, Petra'
'Mitzel, Norbert W.'
_publ_section_title
;
 Hemi- and holo-directed lead(II) complexes in a soft ligand environment.
;
_journal_issue                   3
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              924
_journal_page_last               937
_journal_paper_doi               10.1039/c4dt01406e
_journal_volume                  44
_journal_year                    2015
_chemical_formula_moiety         'C12 H20 N14 O6 Pb S4'
_chemical_formula_sum            'C12 H20 N14 O6 Pb S4'
_chemical_formula_weight         791.85
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      tetragonal
_space_group_IT_number           82
_space_group_name_Hall           'I -4'
_space_group_name_H-M_alt        'I -4'
_symmetry_space_group_name_Hall  'I -4'
_symmetry_space_group_name_H-M   'I -4'
_atom_sites_solution_hydrogens   difmap
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   10.5430(11)
_cell_length_b                   10.5430(11)
_cell_length_c                   11.7670(6)
_cell_measurement_reflns_used    165
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      21.552
_cell_measurement_theta_min      5.626
_cell_volume                     1308.0(2)
_computing_cell_refinement
'Dirax/lsq (Duisenberg & Schreurs, 1989-2000)'
_computing_data_collection       'Collect, Bruker AXS, 2004'
_computing_data_reduction
'EVALCCD (Duisenberg,1998,Thesis.Utrecht University.'
_computing_molecular_graphics    'SHELXTL-PLUS (1990)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       CCD
_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  0.0373
_diffrn_reflns_av_unetI/netI     0.0315
_diffrn_reflns_Laue_measured_fraction_full 0.987
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            13152
_diffrn_reflns_point_group_measured_fraction_full 0.953
_diffrn_reflns_point_group_measured_fraction_max 0.953
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.966
_diffrn_reflns_theta_min         3.865
_exptl_absorpt_coefficient_mu    6.827
_exptl_absorpt_correction_T_max  1.000000
_exptl_absorpt_correction_T_min  0.690436
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS - Bruker Nonius area detector scaling and absorption correction - V2.10'
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    2.011
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       fragment
_exptl_crystal_F_000             768
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.280
_exptl_crystal_size_min          0.280
_refine_diff_density_max         0.780
_refine_diff_density_min         -0.739
_refine_diff_density_rms         0.066
_refine_ls_abs_structure_details
;
 Flack x determined using 819 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   0.066(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.965
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     105
_refine_ls_number_reflns         1804
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.965
_refine_ls_R_factor_all          0.0130
_refine_ls_R_factor_gt           0.0130
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     'w=1/[σ²(Fo²)] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0284
_refine_ls_wR_factor_ref         0.0284
_reflns_Friedel_coverage         0.831
_reflns_Friedel_fraction_full    0.914
_reflns_Friedel_fraction_max     0.911
_reflns_number_gt                1804
_reflns_number_total             1804
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c4dt01406e1.cif
_cod_data_source_block           compound6
_cod_depositor_comments
'Adding full bibliography for 7031671--7031680.cif.'
_cod_original_cell_volume        1308.0(3)
_cod_database_code               7031676
#BEGIN Tags that were not found in dictionaries:
_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.
;
_shelx_estimated_absorpt_t_min   0.234
_shelx_estimated_absorpt_t_max   0.251
_shelxl_version_number           2013-3
#END Tags that were not found in dictionaries
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z'
'y, -x, -z'
'-y, x, -z'
'x+1/2, y+1/2, z+1/2'
'-x+1/2, -y+1/2, z+1/2'
'y+1/2, -x+1/2, -z+1/2'
'-y+1/2, x+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
Pb1 Pb 0.0000 0.0000 0.0000 0.00883(5) Uani 1 4 d S T P
S1 S -0.08438(7) 0.26568(7) 0.05907(6) 0.01394(14) Uani 1 1 d . . .
N1 N 0.0417(2) 0.3505(2) -0.1289(2) 0.0118(5) Uani 1 1 d . . .
H1 H -0.013(4) 0.329(4) -0.182(4) 0.020(10) Uiso 1 1 d . . .
N2 N 0.1542(3) 0.4032(3) -0.1626(3) 0.0133(6) Uani 1 1 d . . .
N3 N 0.1495(2) 0.3757(2) 0.02297(18) 0.0115(6) Uani 1 1 d . . .
N4 N 0.0000 0.0000 0.2671(2) 0.0115(5) Uani 1 2 d S T P
O1 O 0.1014(2) 0.0159(2) 0.21261(19) 0.0195(5) Uani 1 1 d . . .
O2 O 0.0000 0.0000 0.37305(19) 0.0192(5) Uani 1 2 d S T P
C1 C 0.0357(3) 0.3313(3) -0.0164(3) 0.0107(7) Uani 1 1 d . . .
C2 C 0.2176(3) 0.4181(3) -0.0681(3) 0.0139(6) Uani 1 1 d . . .
H2 H 0.300(4) 0.450(4) -0.068(4) 0.021(10) Uiso 1 1 d . . .
C3 C 0.1904(4) 0.3725(5) 0.1412(4) 0.0229(9) Uani 1 1 d . . .
H3A H 0.151(6) 0.430(6) 0.190(5) 0.045(18) Uiso 1 1 d . . .
H3B H 0.179(5) 0.292(6) 0.172(4) 0.044(15) Uiso 1 1 d . . .
H3C H 0.275(7) 0.385(6) 0.147(5) 0.054(17) Uiso 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'
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
O1 Pb1 O1 46.77(9) 3 4
O1 Pb1 O1 147.40(6) 3 2
O1 Pb1 O1 147.40(6) 4 2
O1 Pb1 O1 147.40(6) 3 .
O1 Pb1 O1 147.40(6) 4 .
O1 Pb1 O1 46.77(9) 2 .
O1 Pb1 S1 126.38(5) 3 .
O1 Pb1 S1 80.18(5) 4 .
O1 Pb1 S1 74.36(6) 2 .
O1 Pb1 S1 81.20(6) . .
O1 Pb1 S1 74.36(6) 3 4
O1 Pb1 S1 81.20(6) 4 4
O1 Pb1 S1 80.18(5) 2 4
O1 Pb1 S1 126.38(5) . 4
S1 Pb1 S1 93.037(6) . 4
O1 Pb1 S1 81.20(6) 3 3
O1 Pb1 S1 74.36(6) 4 3
O1 Pb1 S1 126.38(5) 2 3
O1 Pb1 S1 80.18(5) . 3
S1 Pb1 S1 93.036(6) . 3
S1 Pb1 S1 153.39(3) 4 3
O1 Pb1 S1 80.18(5) 3 2
O1 Pb1 S1 126.38(5) 4 2
O1 Pb1 S1 81.20(6) 2 2
O1 Pb1 S1 74.36(6) . 2
S1 Pb1 S1 153.39(3) . 2
S1 Pb1 S1 93.037(6) 4 2
S1 Pb1 S1 93.037(6) 3 2
C1 S1 Pb1 92.17(10) . .
C1 N1 N2 112.9(3) . .
C1 N1 H1 129(3) . .
N2 N1 H1 118(3) . .
C2 N2 N1 104.2(3) . .
C2 N3 C1 107.9(2) . .
C2 N3 C3 127.0(3) . .
C1 N3 C3 125.1(3) . .
O2 N4 O1 120.67(14) . 2
O2 N4 O1 120.67(14) . .
O1 N4 O1 118.7(3) 2 .
N4 O1 Pb1 97.28(16) . .
N1 C1 N3 103.9(3) . .
N1 C1 S1 128.0(2) . .
N3 C1 S1 128.1(3) . .
N2 C2 N3 111.1(3) . .
N2 C2 H2 122(3) . .
N3 C2 H2 127(3) . .
N3 C3 H3A 116(4) . .
N3 C3 H3B 111(3) . .
H3A C3 H3B 107(5) . .
N3 C3 H3C 111(4) . .
H3A C3 H3C 107(6) . .
H3B C3 H3C 103(5) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Pb1 O1 2.726(2) 3
Pb1 O1 2.726(2) 4
Pb1 O1 2.726(2) 2
Pb1 O1 2.726(2) .
Pb1 S1 3.0200(8) .
Pb1 S1 3.0200(8) 4
Pb1 S1 3.0200(8) 3
Pb1 S1 3.0200(8) 2
S1 C1 1.694(3) .
N1 C1 1.340(4) .
N1 N2 1.368(4) .
N1 H1 0.88(5) .
N2 C2 1.307(5) .
N3 C2 1.365(4) .
N3 C1 1.369(4) .
N3 C3 1.457(5) .
N4 O2 1.246(4) .
N4 O1 1.258(2) 2
N4 O1 1.258(2) .
C2 H2 0.93(5) .
C3 H3A 0.93(6) .
C3 H3B 0.93(6) .
C3 H3C 0.91(7) .
