#------------------------------------------------------------------------------
#$Date: 2016-02-18 14:25:00 +0200 (Thu, 18 Feb 2016) $
#$Revision: 176728 $
#$URL: svn://www.crystallography.net/cod/cif/8/10/17/8101701.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_8101701
loop_
_publ_author_name
'B.-S. Zhang'
_publ_section_title
;
Crystal structure of bis[μ-chloro(2,2'-bipyridine-N,N')(μ-
2-chlorobenzoato)lead(II)], [Pb(Cl)(C₁₀H₈N₂)(ClC₆H₄COO)]
₂
;
_journal_issue                   1
_journal_name_full
'Zeitschrift für Kristallographie - New Crystal Structures'
_journal_page_first              73
_journal_page_last               74
_journal_volume                  220
_journal_year                    2005
_chemical_formula_sum            'C17 H12 Cl2 N2 O2 Pb'
_chemical_formula_weight         554.38
_chemical_name_systematic
; 
 bis[mue-chloro(2,2'-bipyridine-N,N')(2-chloro-benzoato)lead(II)]
;
_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                95.55(3)
_cell_angle_beta                 91.46(3)
_cell_angle_gamma                92.36(3)
_cell_formula_units_Z            2
_cell_length_a                   8.5229(17)
_cell_length_b                   9.5084(19)
_cell_length_c                   10.709(2)
_cell_measurement_temperature    293(2)
_cell_volume                     862.7(3)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.956
_diffrn_measured_fraction_theta_max 0.956
_diffrn_measurement_device_type  'Bruker SMART APEX CCD II'
_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  0.0288
_diffrn_reflns_av_sigmaI/netI    0.0344
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            14933
_diffrn_reflns_theta_full        30.52
_diffrn_reflns_theta_max         30.52
_diffrn_reflns_theta_min         2.39
_exptl_absorpt_coefficient_mu    10.099
_exptl_absorpt_correction_T_max  0.3072
_exptl_absorpt_correction_T_min  0.1629
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.134
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             520
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.997
_refine_diff_density_min         -0.993
_refine_diff_density_rms         0.108
_refine_ls_extinction_coef       0.0003(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     218
_refine_ls_number_reflns         5055
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.0334
_refine_ls_R_factor_gt           0.0253
_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)+(0.0285P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0548
_refine_ls_wR_factor_ref         0.0565
_reflns_number_gt                4310
_reflns_number_total             5055
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            1267-1431.cff
_cod_data_source_block           shx97
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               8101701
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_Wyckoff_symbol
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Pb1 Pb 0.242325(13) 0.914817(12) 0.473404(12) 0.03684(6) Uani 1 2 i d . . .
N1 N 0.2834(3) 0.6678(3) 0.5309(3) 0.0423(7) Uani 1 2 i d . . .
N2 N 0.0864(3) 0.7213(3) 0.3405(3) 0.0392(6) Uani 1 2 i d . . .
O1 O 0.3988(4) 0.8270(3) 0.2976(3) 0.0788(10) Uani 1 2 i d . . .
O2 O 0.5293(4) 1.0298(4) 0.3384(3) 0.0695(9) Uani 1 2 i d . . .
Cl1 Cl 0.3821(2) 0.6670(2) 0.06604(19) 0.1169(6) Uani 1 2 i d . . .
Cl2 Cl -0.02149(12) 0.89287(10) 0.64424(10) 0.0506(2) Uani 1 2 i d . . .
C1 C 0.3771(5) 0.6465(5) 0.6296(4) 0.0544(10) Uani 1 2 i d . . .
H1 H 0.4250 0.7242 0.6774 0.088 Uiso 1 2 i calc R . .
C2 C 0.4041(6) 0.5117(5) 0.6620(5) 0.0677(13) Uani 1 2 i d . . .
H2 H 0.4699 0.4989 0.7303 0.088 Uiso 1 2 i calc R . .
C3 C 0.3329(5) 0.3982(5) 0.5923(5) 0.0655(12) Uani 1 2 i d . . .
H3 H 0.3498 0.3070 0.6126 0.088 Uiso 1 2 i calc R . .
C4 C 0.2362(4) 0.4190(4) 0.4921(4) 0.0543(10) Uani 1 2 i d . . .
H4 H 0.1859 0.3424 0.4445 0.088 Uiso 1 2 i calc R . .
C5 C 0.2142(4) 0.5567(4) 0.4624(4) 0.0386(7) Uani 1 2 i d . . .
C6 C 0.1133(4) 0.5847(4) 0.3541(3) 0.0387(7) Uani 1 2 i d . . .
C7 C 0.0465(5) 0.4767(4) 0.2708(4) 0.0525(9) Uani 1 2 i d . . .
H7 H 0.0647 0.3829 0.2818 0.088 Uiso 1 2 i calc R . .
C8 C -0.0468(5) 0.5093(5) 0.1716(4) 0.0630(11) Uani 1 2 i d . . .
H8 H -0.0923 0.4379 0.1152 0.088 Uiso 1 2 i calc R . .
C9 C -0.0718(5) 0.6484(5) 0.1572(4) 0.0577(10) Uani 1 2 i d . . .
H9 H -0.1335 0.6731 0.0906 0.088 Uiso 1 2 i calc R . .
C10 C -0.0037(4) 0.7499(4) 0.2433(4) 0.0493(9) Uani 1 2 i d . . .
H10 H -0.0212 0.8441 0.2335 0.088 Uiso 1 2 i calc R . .
C11 C 0.4953(4) 0.9203(4) 0.2686(4) 0.0433(8) Uani 1 2 i d . . .
C12 C 0.5749(4) 0.8945(4) 0.1452(4) 0.0463(9) Uani 1 2 i d . . .
C13 C 0.6967(5) 0.9887(6) 0.1200(5) 0.0659(13) Uani 1 2 i d . . .
H13 H 0.7266 1.0631 0.1798 0.088 Uiso 1 2 i calc R . .
C14 C 0.7739(6) 0.9742(9) 0.0084(7) 0.098(2) Uani 1 2 i d . . .
H14 H 0.8545 1.0386 -0.0070 0.088 Uiso 1 2 i calc R . .
C15 C 0.7315(9) 0.8653(11) -0.0788(6) 0.117(3) Uani 1 2 i d . . .
H15 H 0.7843 0.8550 -0.1539 0.088 Uiso 1 2 i calc R . .
C16 C 0.6115(8) 0.7698(8) -0.0580(5) 0.095(2) Uani 1 2 i d . . .
H16 H 0.5835 0.6959 -0.1188 0.088 Uiso 1 2 i calc R . .
C17 C 0.5319(5) 0.7838(5) 0.0542(4) 0.0631(12) Uani 1 2 i 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'
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
_geom_angle_publ_flag
O1 Pb1 N1 80.38(11) . . ?
O1 Pb1 N2 70.69(11) . . ?
N1 Pb1 N2 64.93(10) . . ?
O1 Pb1 Cl2 152.92(8) . . ?
N1 Pb1 Cl2 81.78(7) . . ?
N2 Pb1 Cl2 83.34(7) . . ?
O1 Pb1 Cl2 102.95(10) . 2_576 ?
N1 Pb1 Cl2 145.93(7) . 2_576 ?
N2 Pb1 Cl2 83.93(7) . 2_576 ?
Cl2 Pb1 Cl2 81.16(4) . 2_576 ?
C5 N1 C1 119.3(3) . . ?
C5 N1 Pb1 120.2(2) . . ?
C1 N1 Pb1 120.4(3) . . ?
C10 N2 C6 118.2(3) . . ?
C10 N2 Pb1 121.3(2) . . ?
C6 N2 Pb1 119.7(2) . . ?
C11 O1 Pb1 111.3(3) . . ?
Pb1 Cl2 Pb1 98.84(4) . 2_576 ?
N1 C1 C2 121.7(4) . . ?
N1 C1 H1 119.2 . . ?
C2 C1 H1 119.2 . . ?
C3 C2 C1 119.0(4) . . ?
C3 C2 H2 120.5 . . ?
C1 C2 H2 120.5 . . ?
C2 C3 C4 119.7(4) . . ?
C2 C3 H3 120.1 . . ?
C4 C3 H3 120.1 . . ?
C3 C4 C5 119.1(4) . . ?
C3 C4 H4 120.4 . . ?
C5 C4 H4 120.4 . . ?
N1 C5 C4 121.2(3) . . ?
N1 C5 C6 117.6(3) . . ?
C4 C5 C6 121.2(3) . . ?
N2 C6 C7 121.0(3) . . ?
N2 C6 C5 116.8(3) . . ?
C7 C6 C5 122.2(3) . . ?
C8 C7 C6 119.6(4) . . ?
C8 C7 H7 120.2 . . ?
C6 C7 H7 120.2 . . ?
C9 C8 C7 119.2(4) . . ?
C9 C8 H8 120.4 . . ?
C7 C8 H8 120.4 . . ?
C10 C9 C8 118.3(4) . . ?
C10 C9 H9 120.8 . . ?
C8 C9 H9 120.8 . . ?
N2 C10 C9 123.7(4) . . ?
N2 C10 H10 118.1 . . ?
C9 C10 H10 118.1 . . ?
O2 C11 O1 122.6(4) . . ?
O2 C11 C12 119.7(3) . . ?
O1 C11 C12 117.6(4) . . ?
C13 C12 C17 118.3(4) . . ?
C13 C12 C11 117.7(4) . . ?
C17 C12 C11 123.9(4) . . ?
C14 C13 C12 121.5(6) . . ?
C14 C13 H13 119.3 . . ?
C12 C13 H13 119.3 . . ?
C15 C14 C13 119.5(7) . . ?
C15 C14 H14 120.2 . . ?
C13 C14 H14 120.2 . . ?
C14 C15 C16 121.0(6) . . ?
C14 C15 H15 119.5 . . ?
C16 C15 H15 119.5 . . ?
C15 C16 C17 120.0(6) . . ?
C15 C16 H16 120.0 . . ?
C17 C16 H16 120.0 . . ?
C16 C17 C12 119.6(5) . . ?
C16 C17 Cl1 115.8(5) . . ?
C12 C17 Cl1 124.5(3) . . ?
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
Pb1 O1 2.436(3) . ?
Pb1 N1 2.521(3) . ?
Pb1 N2 2.524(3) . ?
Pb1 Cl2 2.9480(13) . ?
Pb1 Cl2 3.0137(13) 2_576 ?
N1 C5 1.334(5) . ?
N1 C1 1.345(5) . ?
N2 C10 1.333(5) . ?
N2 C6 1.349(4) . ?
O1 C11 1.251(5) . ?
O2 C11 1.241(5) . ?
Cl1 C17 1.673(6) . ?
Cl2 Pb1 3.0137(13) 2_576 ?
C1 C2 1.387(6) . ?
C1 H1 0.9300 . ?
C2 C3 1.363(7) . ?
C2 H2 0.9300 . ?
C3 C4 1.371(6) . ?
C3 H3 0.9300 . ?
C4 C5 1.395(5) . ?
C4 H4 0.9300 . ?
C5 C6 1.478(5) . ?
C6 C7 1.386(5) . ?
C7 C8 1.378(6) . ?
C7 H7 0.9300 . ?
C8 C9 1.370(6) . ?
C8 H8 0.9300 . ?
C9 C10 1.368(6) . ?
C9 H9 0.9300 . ?
C10 H10 0.9300 . ?
C11 C12 1.504(5) . ?
C12 C13 1.393(6) . ?
C12 C17 1.393(6) . ?
C13 C14 1.376(7) . ?
C13 H13 0.9300 . ?
C14 C15 1.357(13) . ?
C14 H14 0.9300 . ?
C15 C16 1.377(11) . ?
C15 H15 0.9300 . ?
C16 C17 1.393(7) . ?
C16 H16 0.9300 . ?
