#------------------------------------------------------------------------------
#$Date: 2016-03-23 00:23:57 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179108 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/70/4307058.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_4307058
loop_
_publ_author_name
'Krzysztof Lyczko'
'Wojciech Starosta'
'Ingmar Persson'
_publ_contact_author_address
;Institute of Nuclear Chemistry and Technology
03-195 Warsaw, Dorodna 16
Poland
;
_publ_contact_author_email       kml@ichtj.waw.pl
_publ_contact_author_name        'Lyczko K.'
_publ_section_title
;
Influence of pH and Counteranion on the Structure of Tropolonato-Lead(II)
Complexes: Structural and Infrared Characterization of Formed Lead
Compounds
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4402
_journal_page_last               4410
_journal_paper_doi               10.1021/ic061561f
_journal_volume                  46
_journal_year                    2007
_chemical_formula_sum            'C14 H10 O4 Pb'
_chemical_formula_weight         449.41
_chemical_name_common            bis(Tropolonato)-lead(II)
_chemical_name_systematic
; 
bis((μ₂-Tropolonato-O,O,O')-(tropolonato-O,O')-lead(II)) 
;
_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                 95.67(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   4.9520(10)
_cell_length_b                   10.753(2)
_cell_length_c                   23.947(5)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      15
_cell_measurement_theta_min      6
_cell_volume                     1268.9(4)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.896
_diffrn_measured_fraction_theta_max 0.757
_diffrn_measurement_device_type  'KUMA KM-4 four circle diffractometer'
_diffrn_measurement_method       'profile data from ω/2θ scan'
_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  0.0585
_diffrn_reflns_av_sigmaI/netI    0.0651
_diffrn_reflns_limit_h_max       0
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            2676
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         28.43
_diffrn_reflns_theta_min         1.71
_diffrn_standards_decay_%        4.20
_diffrn_standards_interval_count 200
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    13.302
_exptl_absorpt_correction_T_max  0.35094
_exptl_absorpt_correction_T_min  0.04965
_exptl_absorpt_correction_type   analytical
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.353
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             832
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.06
_refine_diff_density_max         2.610
_refine_diff_density_min         -2.555
_refine_diff_density_rms         0.400
_refine_ls_extinction_coef       0.0013(7)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.088
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     173
_refine_ls_number_reflns         2423
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.088
_refine_ls_R_factor_all          0.1091
_refine_ls_R_factor_gt           0.0661
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.1496P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1893
_refine_ls_wR_factor_ref         0.2092
_reflns_number_gt                1620
_reflns_number_total             2423
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic061561f-file002_1.cif
_cod_data_source_block           Pbtrop4
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4307058
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
Pb1 Pb -0.13768(14) 0.65510(6) 0.05050(3) 0.0433(3) Uani 1 1 d . . .
O1 O 0.227(3) 0.5963(13) 0.1142(6) 0.059(4) Uani 1 1 d . . .
C1 C 0.290(4) 0.6638(17) 0.1557(8) 0.050(5) Uani 1 1 d . . .
C2 C 0.131(4) 0.7791(16) 0.1617(9) 0.051(5) Uani 1 1 d . . .
C7 C 0.519(4) 0.621(2) 0.1943(11) 0.066(6) Uani 1 1 d . . .
H7 H 0.6031 0.5489 0.1834 0.079 Uiso 1 1 calc R . .
O2 O -0.049(3) 0.8015(12) 0.1251(7) 0.061(4) Uani 1 1 d . . .
C3 C 0.206(5) 0.8646(16) 0.2077(10) 0.055(5) Uani 1 1 d . . .
H3 H 0.1019 0.9367 0.2046 0.067 Uiso 1 1 calc R . .
C6 C 0.629(5) 0.671(2) 0.2441(10) 0.064(6) Uani 1 1 d . . .
H6 H 0.7637 0.6218 0.2628 0.077 Uiso 1 1 calc R . .
C4 C 0.387(4) 0.8669(17) 0.2538(9) 0.050(5) Uani 1 1 d . . .
H4 H 0.3828 0.9365 0.2768 0.060 Uiso 1 1 calc R . .
O12 O 0.178(2) 0.6009(10) -0.0140(6) 0.046(3) Uani 1 1 d . . .
O11 O 0.035(3) 0.8246(11) 0.0076(7) 0.057(4) Uani 1 1 d . . .
C12 C 0.285(3) 0.6859(15) -0.0397(8) 0.038(4) Uani 1 1 d . . .
C11 C 0.191(4) 0.8130(16) -0.0281(9) 0.048(5) Uani 1 1 d . . .
C5 C 0.582(5) 0.775(3) 0.2710(11) 0.074(7) Uani 1 1 d . . .
H5 H 0.6884 0.7899 0.3045 0.089 Uiso 1 1 calc R . .
C13 C 0.479(4) 0.6557(15) -0.0765(8) 0.042(4) Uani 1 1 d . . .
H13 H 0.5157 0.5709 -0.0776 0.050 Uiso 1 1 calc R . .
C15 C 0.613(4) 0.8506(17) -0.1202(11) 0.056(5) Uani 1 1 d . . .
H15 H 0.7266 0.8811 -0.1456 0.067 Uiso 1 1 calc R . .
C17 C 0.268(5) 0.9229(16) -0.0548(8) 0.059(6) Uani 1 1 d . . .
H17 H 0.1864 0.9956 -0.0436 0.071 Uiso 1 1 calc R . .
C14 C 0.629(4) 0.7249(19) -0.1114(9) 0.055(5) Uani 1 1 d . . .
H14 H 0.7522 0.6815 -0.1309 0.066 Uiso 1 1 calc R . .
C16 C 0.456(5) 0.9385(16) -0.0975(11) 0.062(6) Uani 1 1 d . . .
H16 H 0.4721 1.0190 -0.1111 0.074 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'
O O 0.0106 0.0060 '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
O11 Pb1 O1 102.0(6) . . ?
O11 Pb1 O12 66.8(4) . . ?
O1 Pb1 O12 80.9(5) . . ?
O11 Pb1 O2 76.3(5) . . ?
O1 Pb1 O2 67.5(4) . . ?
O12 Pb1 O2 124.3(5) . . ?
C1 O1 Pb1 118.6(11) . . ?
O1 C1 C7 115.9(17) . . ?
O1 C1 C2 118.3(18) . . ?
C7 C1 C2 125.9(19) . . ?
O2 C2 C3 122.4(17) . . ?
O2 C2 C1 117.1(18) . . ?
C3 C2 C1 120(2) . . ?
C6 C7 C1 130(2) . . ?
C6 C7 H7 115.0 . . ?
C1 C7 H7 115.0 . . ?
C2 O2 Pb1 118.5(11) . . ?
C4 C3 C2 136.8(19) . . ?
C4 C3 H3 111.6 . . ?
C2 C3 H3 111.6 . . ?
C5 C6 C7 133(2) . . ?
C5 C6 H6 113.6 . . ?
C7 C6 H6 113.6 . . ?
C3 C4 C5 127.2(19) . . ?
C3 C4 H4 116.4 . . ?
C5 C4 H4 116.4 . . ?
C12 O12 Pb1 118.6(10) . . ?
C11 O11 Pb1 121.6(11) . . ?
O12 C12 C13 119.3(15) . . ?
O12 C12 C11 115.4(16) . . ?
C13 C12 C11 125.3(17) . . ?
O11 C11 C17 116.8(17) . . ?
O11 C11 C12 117.3(17) . . ?
C17 C11 C12 125.9(19) . . ?
C6 C5 C4 127(2) . . ?
C6 C5 H5 116.7 . . ?
C4 C5 H5 116.7 . . ?
C14 C13 C12 133.9(17) . . ?
C14 C13 H13 113.1 . . ?
C12 C13 H13 113.1 . . ?
C16 C15 C14 130(2) . . ?
C16 C15 H15 114.8 . . ?
C14 C15 H15 114.8 . . ?
C11 C17 C16 129.1(18) . . ?
C11 C17 H17 115.4 . . ?
C16 C17 H17 115.4 . . ?
C15 C14 C13 127(2) . . ?
C15 C14 H14 116.7 . . ?
C13 C14 H14 116.7 . . ?
C15 C16 C17 128.7(17) . . ?
C15 C16 H16 115.7 . . ?
C17 C16 H16 115.7 . . ?
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 O11 2.298(13) . ?
Pb1 O1 2.335(14) . ?
Pb1 O12 2.375(13) . ?
Pb1 O2 2.389(14) . ?
O1 C1 1.24(2) . ?
C1 C7 1.47(3) . ?
C1 C2 1.48(2) . ?
C2 O2 1.21(3) . ?
C2 C3 1.46(3) . ?
C7 C6 1.37(3) . ?
C7 H7 0.9300 . ?
C3 C4 1.35(3) . ?
C3 H3 0.9300 . ?
C6 C5 1.33(3) . ?
C6 H6 0.9300 . ?
C4 C5 1.41(3) . ?
C4 H4 0.9300 . ?
O12 C12 1.25(2) . ?
O11 C11 1.22(2) . ?
C12 C13 1.41(3) . ?
C12 C11 1.48(2) . ?
C11 C17 1.41(3) . ?
C5 H5 0.9300 . ?
C13 C14 1.39(3) . ?
C13 H13 0.9300 . ?
C15 C16 1.37(3) . ?
C15 C14 1.37(3) . ?
C15 H15 0.9300 . ?
C17 C16 1.46(3) . ?
C17 H17 0.9300 . ?
C14 H14 0.9300 . ?
C16 H16 0.9300 . ?
