#------------------------------------------------------------------------------
#$Date: 2016-02-21 02:03:34 +0200 (Sun, 21 Feb 2016) $
#$Revision: 176798 $
#$URL: svn://www.crystallography.net/cod/cif/2/23/03/2230348.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2230348
loop_
_publ_author_name
'Appleton, Sarah E.'
'Briand, Glen G.'
'Decken, Andreas'
'Smith, Anita S.'
_publ_section_title
;
 catena-Poly[[bis(pyridine)lead(II)]bis(μ-pentafluorobenzenethiolato)]
;
_journal_coeditor_code           HG5027
_journal_issue                   6
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m714
_journal_paper_doi               10.1107/S160053681101659X
_journal_volume                  67
_journal_year                    2011
_chemical_formula_iupac          '[Pb (C6 F5 S)2 C5 H5 N)2]'
_chemical_formula_moiety         'C22 H10 F10 N2 Pb S2'
_chemical_formula_sum            'C22 H10 F10 N2 Pb S2'
_chemical_formula_weight         763.63
_chemical_name_systematic
;
catena-Poly[[bis(pyridine)lead(II)]bis(μ-pentafluorobenzenethiolato)]
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 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                 111.339(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   19.9288(19)
_cell_length_b                   5.0416(5)
_cell_length_c                   24.9155(19)
_cell_measurement_reflns_used    5261
_cell_measurement_temperature    198.0(10)
_cell_measurement_theta_max      27.917
_cell_measurement_theta_min      2.1945
_cell_volume                     2331.7(4)
_computing_cell_refinement       'SAINT (Bruker, 2006)'
_computing_data_collection       'SMART (Bruker, 1999)'
_computing_data_reduction        'SAINT (Bruker, 2006)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008b)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008b)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008b)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008b)'
_diffrn_ambient_temperature      198.0(10)
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.960
_diffrn_measurement_device_type  'Bruker SMART1000/P4'
_diffrn_measurement_method       'φ and ω'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0546
_diffrn_reflns_av_sigmaI/netI    0.0581
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            6756
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         27.49
_diffrn_reflns_theta_min         4.19
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    7.510
_exptl_absorpt_correction_T_max  0.5205
_exptl_absorpt_correction_T_min  0.0986
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2008a)'
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    2.175
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Parallelepiped
_exptl_crystal_F_000             1440
_exptl_crystal_size_max          0.57
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_refine_diff_density_max         3.834
_refine_diff_density_min         -2.705
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     168
_refine_ls_number_reflns         2575
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.055
_refine_ls_R_factor_all          0.0422
_refine_ls_R_factor_gt           0.0402
_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)+(0.0608P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0956
_refine_ls_wR_factor_ref         0.0966
_reflns_number_gt                2421
_reflns_number_total             2575
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            hg5027.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               2230348
_cod_database_fobs_code          2230348
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'
loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_disorder_assembly
_atom_site_disorder_group
Pb Pb 0.0000 0.57741(4) 0.2500 0.02457(12) Uani d S 1 2 . .
S S1 -0.00240(9) 0.9584(2) 0.17593(6) 0.0308(3) Uani d . 1 1 . .
F F2 -0.1488(2) 0.9328(7) 0.0811(2) 0.0491(11) Uani d . 1 1 . .
F F3 -0.1937(2) 0.5959(8) -0.0085(2) 0.0643(15) Uani d . 1 1 . .
F F4 -0.1038(2) 0.2260(7) -0.02233(17) 0.0513(10) Uani d . 1 1 . .
F F5 0.03376(19) 0.1979(7) 0.05311(15) 0.0416(8) Uani d . 1 1 . .
F F6 0.0806(2) 0.5350(7) 0.14221(17) 0.0404(8) Uani d . 1 1 . .
N N1 0.1419(3) 0.5895(8) 0.2954(3) 0.0333(11) Uani d . 1 1 . .
C C1 -0.0321(3) 0.7450(9) 0.1159(2) 0.0261(10) Uani d . 1 1 . .
C C2 -0.1022(3) 0.7539(11) 0.0757(2) 0.0324(11) Uani d . 1 1 . .
C C3 -0.1263(4) 0.5816(11) 0.0295(3) 0.0369(14) Uani d . 1 1 . .
C C4 -0.0802(4) 0.3944(11) 0.0226(3) 0.0341(13) Uani d . 1 1 . .
C C5 -0.0113(3) 0.3793(11) 0.0607(3) 0.0304(12) Uani d . 1 1 . .
C C6 0.0123(3) 0.5558(9) 0.1063(3) 0.0278(11) Uani d . 1 1 . .
C C7 0.1855(3) 0.7571(12) 0.2823(3) 0.0408(13) Uani d . 1 1 . .
H H7 0.1652 0.8817 0.2534 0.049 Uiso calc R 1 1 . .
C C8 0.2590(4) 0.7531(14) 0.3097(3) 0.0512(17) Uani d . 1 1 . .
H H8 0.2880 0.8719 0.2994 0.061 Uiso calc R 1 1 . .
C C9 0.2891(4) 0.5700(12) 0.3528(4) 0.052(2) Uani d . 1 1 . .
H H9 0.3387 0.5646 0.3726 0.062 Uiso calc R 1 1 . .
C C10 0.2453(4) 0.3984(13) 0.3659(4) 0.053(2) Uani d . 1 1 . .
H H10 0.2645 0.2719 0.3946 0.063 Uiso calc R 1 1 . .
C C11 0.1719(4) 0.4119(11) 0.3363(3) 0.0426(16) Uani d . 1 1 . .
H H11 0.1423 0.2918 0.3455 0.051 Uiso calc R 1 1 . .
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'
F F 0.0171 0.0103 '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'
Pb Pb -3.3944 10.1111 '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_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
N1 Pb N1 . 2 177.34(18) ?
N1 Pb S1 . 2 86.55(12) ?
N1 Pb S1 2 2 91.52(12) ?
N1 Pb S1 . . 91.52(12) ?
N1 Pb S1 2 . 86.55(12) ?
S1 Pb S1 2 . 87.18(6) ?
C1 S1 Pb . . 93.67(16) ?
C11 N1 C7 . . 117.6(6) ?
C11 N1 Pb . . 115.3(4) ?
C7 N1 Pb . . 127.0(4) ?
C6 C1 C2 . . 115.9(5) ?
C6 C1 S1 . . 122.1(4) ?
C2 C1 S1 . . 122.0(4) ?
F2 C2 C3 . . 117.8(5) ?
F2 C2 C1 . . 120.1(5) ?
C3 C2 C1 . . 122.1(5) ?
F3 C3 C4 . . 119.8(5) ?
F3 C3 C2 . . 120.7(5) ?
C4 C3 C2 . . 119.5(6) ?
F4 C4 C5 . . 120.3(5) ?
F4 C4 C3 . . 119.4(6) ?
C5 C4 C3 . . 120.3(5) ?
F5 C5 C4 . . 119.8(5) ?
F5 C5 C6 . . 120.7(5) ?
C4 C5 C6 . . 119.5(5) ?
F6 C6 C1 . . 120.1(5) ?
F6 C6 C5 . . 117.3(5) ?
C1 C6 C5 . . 122.7(5) ?
N1 C7 C8 . . 122.8(6) ?
N1 C7 H7 . . 118.6 ?
C8 C7 H7 . . 118.6 ?
C7 C8 C9 . . 118.7(7) ?
C7 C8 H8 . . 120.6 ?
C9 C8 H8 . . 120.6 ?
C10 C9 C8 . . 118.7(7) ?
C10 C9 H9 . . 120.6 ?
C8 C9 H9 . . 120.6 ?
C9 C10 C11 . . 119.6(7) ?
C9 C10 H10 . . 120.2 ?
C11 C10 H10 . . 120.2 ?
N1 C11 C10 . . 122.5(7) ?
N1 C11 H11 . . 118.7 ?
C10 C11 H11 . . 118.7 ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Pb N1 . 2.636(5) ?
Pb N1 2 2.636(5) ?
Pb S1 2 2.6519(14) ?
Pb S1 . 2.6519(14) ?
S1 C1 . 1.761(5) ?
F2 C2 . 1.336(6) ?
F3 C3 . 1.334(8) ?
F4 C4 . 1.345(7) ?
F5 C5 . 1.342(6) ?
F6 C6 . 1.334(7) ?
N1 C11 . 1.326(8) ?
N1 C7 . 1.335(8) ?
C1 C6 . 1.379(8) ?
C1 C2 . 1.392(7) ?
C2 C3 . 1.382(8) ?
C3 C4 . 1.371(8) ?
C4 C5 . 1.359(9) ?
C5 C6 . 1.384(8) ?
C7 C8 . 1.373(8) ?
C7 H7 . 0.9300 ?
C8 C9 . 1.378(11) ?
C8 H8 . 0.9300 ?
C9 C10 . 1.350(12) ?
C9 H9 . 0.9300 ?
C10 C11 . 1.380(10) ?
C10 H10 . 0.9300 ?
C11 H11 . 0.9300 ?
