#------------------------------------------------------------------------------
#$Date: 2016-03-23 00:23:57 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179108 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/70/4307061.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_4307061
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            'C15 H14 N2 O11 Pb2'
_chemical_formula_weight         812.66
_chemical_name_systematic
; 
catena-((μ₃Tropolonato-O,O,O',O')-(μ₂-tropolonato-O,O,O')
(μ₂-nitrato-O,O,O',O'')-(nitrato-O,O')-methanolato-di-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                90.30(3)
_cell_angle_beta                 97.11(3)
_cell_angle_gamma                94.97(3)
_cell_formula_units_Z            2
_cell_length_a                   7.4220(15)
_cell_length_b                   10.171(2)
_cell_length_c                   12.872(3)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      15
_cell_measurement_theta_min      6
_cell_volume                     960.5(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 0.846
_diffrn_measured_fraction_theta_max 0.846
_diffrn_measurement_device_type  'KUMA KM-4 four circles diffractometer'
_diffrn_measurement_method       'profile scan 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  0.0686
_diffrn_reflns_av_sigmaI/netI    0.0601
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            5080
_diffrn_reflns_theta_full        30.06
_diffrn_reflns_theta_max         30.06
_diffrn_reflns_theta_min         1.59
_diffrn_standards_decay_%        27.92
_diffrn_standards_interval_count 200
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    17.570
_exptl_absorpt_correction_T_max  0.09463
_exptl_absorpt_correction_T_min  0.01939
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
analytical, Oxford Diffraction CCD Data Reduction ver. 1.169.8 
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    2.810
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             740
_exptl_crystal_size_max          0.37
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.22
_refine_diff_density_max         4.208
_refine_diff_density_min         -3.059
_refine_diff_density_rms         0.404
_refine_ls_extinction_coef       0.0120(8)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   0.971
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     273
_refine_ls_number_reflns         4765
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.972
_refine_ls_R_factor_all          0.0824
_refine_ls_R_factor_gt           0.0490
_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)+(0.1213P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1374
_refine_ls_wR_factor_ref         0.1521
_reflns_number_gt                3397
_reflns_number_total             4765
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic061561f-file002_4.cif
_cod_data_source_block           Pbtrop3
_cod_original_cell_volume        960.5(3)
_cod_database_code               4307061
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_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Pb1 Pb 0.46074(6) 0.93243(4) 0.33890(3) 0.02694(16) Uani 1 1 d . . .
Pb2 Pb 0.74517(6) 0.97140(4) 0.08782(3) 0.02612(16) Uani 1 1 d . . .
O12 O 0.5102(12) 0.8323(9) -0.0056(6) 0.0297(18) Uani 1 1 d . . .
O11 O 0.6082(12) 0.8149(8) 0.1954(6) 0.0298(18) Uani 1 1 d . . .
O3 O 0.3187(14) 0.9880(9) 0.1448(7) 0.0354(19) Uani 1 1 d . . .
O1 O 0.5509(13) 1.1158(9) 0.4504(6) 0.034(2) Uani 1 1 d . . .
O7 O 0.9909(13) 0.8950(10) 0.2553(7) 0.039(2) Uani 1 1 d . . .
N1 N 0.2408(14) 1.0860(10) 0.1652(7) 0.027(2) Uani 1 1 d . . .
O9 O 0.7555(14) 0.8320(13) 0.4088(7) 0.051(3) Uani 1 1 d D . .
H9 H 0.8055 0.7881 0.3572 0.061 Uiso 1 1 calc RD . .
C11 C 0.5102(15) 0.7159(10) 0.1506(9) 0.022(2) Uani 1 1 d . . .
O5 O 0.2740(14) 1.1425(10) 0.2493(8) 0.040(2) Uani 1 1 d . . .
O6 O 0.9542(14) 0.7826(12) 0.1132(8) 0.047(2) Uani 1 1 d . . .
C12 C 0.4451(16) 0.7267(12) 0.0387(9) 0.027(2) Uani 1 1 d . . .
N2 N 1.0145(14) 0.7945(12) 0.2076(9) 0.034(2) Uani 1 1 d . . .
C17 C 0.476(2) 0.6027(14) 0.2105(10) 0.038(3) Uani 1 1 d . . .
H17 H 0.5354 0.6067 0.2786 0.045 Uiso 1 1 calc R . .
C1 C 0.6443(16) 1.2169(12) 0.4147(8) 0.026(2) Uani 1 1 d . . .
C7 C 0.6538(19) 1.3396(13) 0.4649(10) 0.035(3) Uani 1 1 d . . .
H7 H 0.5869 1.3402 0.5213 0.042 Uiso 1 1 calc R . .
C16 C 0.368(2) 0.4863(16) 0.1839(14) 0.053(4) Uani 1 1 d . . .
H16 H 0.3675 0.4252 0.2374 0.064 Uiso 1 1 calc R . .
C6 C 0.743(2) 1.4603(14) 0.4468(11) 0.041(3) Uani 1 1 d . . .
H6 H 0.7199 1.5300 0.4887 0.049 Uiso 1 1 calc R . .
O2 O 0.6843(12) 1.0742(9) 0.2778(6) 0.0300(18) Uani 1 1 d . . .
O4 O 0.1224(13) 1.1233(10) 0.0962(7) 0.038(2) Uani 1 1 d . . .
C3 C 0.8564(17) 1.2766(13) 0.2784(9) 0.031(2) Uani 1 1 d . . .
H3 H 0.9122 1.2407 0.2253 0.037 Uiso 1 1 calc R . .
C2 C 0.7294(16) 1.1881(12) 0.3200(9) 0.027(2) Uani 1 1 d . . .
C4 C 0.913(2) 1.4060(17) 0.3017(11) 0.045(3) Uani 1 1 d . . .
H4 H 0.9992 1.4437 0.2617 0.054 Uiso 1 1 calc R . .
C14 C 0.2407(19) 0.5149(15) 0.0029(13) 0.043(3) Uani 1 1 d . . .
H14 H 0.1556 0.4760 -0.0499 0.052 Uiso 1 1 calc R . .
C13 C 0.3277(18) 0.6337(14) -0.0194(10) 0.035(3) Uani 1 1 d . . .
H13 H 0.3018 0.6568 -0.0892 0.042 Uiso 1 1 calc R . .
C5 C 0.860(2) 1.4909(13) 0.3769(12) 0.047(4) Uani 1 1 d . . .
H5 H 0.9116 1.5777 0.3784 0.057 Uiso 1 1 calc R . .
C15 C 0.266(2) 0.4467(16) 0.0948(13) 0.051(4) Uani 1 1 d . . .
H15 H 0.2035 0.3633 0.0949 0.061 Uiso 1 1 calc R . .
O8 O 1.1043(19) 0.7114(13) 0.2532(12) 0.072(4) Uani 1 1 d . . .
C9 C 0.856(2) 0.828(2) 0.5057(13) 0.058(4) Uani 1 1 d . . .
H92 H 0.9028 0.9165 0.5279 0.087 Uiso 1 1 calc R . .
H93 H 0.9562 0.7754 0.5016 0.087 Uiso 1 1 calc R . .
H91 H 0.7806 0.7910 0.5552 0.087 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
Pb Pb -3.3944 10.1111 '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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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'
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
O2 Pb1 O1 67.4(3) . . ?
O2 Pb1 O9 76.9(3) . . ?
O1 Pb1 O9 89.1(4) . . ?
O2 Pb1 O11 69.8(3) . . ?
O1 Pb1 O11 134.5(3) . . ?
O9 Pb1 O11 66.5(3) . . ?
O2 Pb1 O3 75.9(3) . . ?
O1 Pb1 O3 115.4(3) . . ?
O9 Pb1 O3 131.8(3) . . ?
O11 Pb1 O3 67.0(3) . . ?
O12 Pb2 O11 67.3(3) . . ?
O12 Pb2 O6 91.8(3) . . ?
O11 Pb2 O6 73.0(3) . . ?
C12 O12 Pb2 119.4(7) . . ?
C11 O11 Pb2 117.8(7) . . ?
C11 O11 Pb1 114.7(7) . . ?
Pb2 O11 Pb1 110.5(3) . . ?
N1 O3 Pb1 98.8(7) . . ?
C1 O1 Pb1 118.5(7) . . ?
O5 N1 O3 121.5(11) . . ?
O5 N1 O4 120.9(11) . . ?
O3 N1 O4 117.6(10) . . ?
C9 O9 Pb1 134.3(10) . . ?
C9 O9 H9 112.9 . . ?
Pb1 O9 H9 112.9 . . ?
O11 C11 C17 118.4(11) . . ?
O11 C11 C12 117.3(10) . . ?
C17 C11 C12 124.3(11) . . ?
N2 O6 Pb2 102.3(8) . . ?
O12 C12 C13 120.3(11) . . ?
O12 C12 C11 114.9(10) . . ?
C13 C12 C11 124.8(11) . . ?
O8 N2 O7 119.0(13) . . ?
O8 N2 O6 121.9(14) . . ?
O7 N2 O6 119.0(12) . . ?
C16 C17 C11 130.3(14) . . ?
C16 C17 H17 114.8 . . ?
C11 C17 H17 114.8 . . ?
O1 C1 C7 119.7(10) . . ?
O1 C1 C2 114.6(10) . . ?
C7 C1 C2 125.7(11) . . ?
C6 C7 C1 132.3(12) . . ?
C6 C7 H7 113.8 . . ?
C1 C7 H7 113.8 . . ?
C15 C16 C17 131.2(16) . . ?
C15 C16 H16 114.4 . . ?
C17 C16 H16 114.4 . . ?
C5 C6 C7 128.9(13) . . ?
C5 C6 H6 115.6 . . ?
C7 C6 H6 115.6 . . ?
C2 O2 Pb1 120.7(7) . . ?
C4 C3 C2 131.6(12) . . ?
C4 C3 H3 114.2 . . ?
C2 C3 H3 114.2 . . ?
O2 C2 C3 120.4(10) . . ?
O2 C2 C1 116.0(10) . . ?
C3 C2 C1 123.6(11) . . ?
C3 C4 C5 129.9(13) . . ?
C3 C4 H4 115.0 . . ?
C5 C4 H4 115.0 . . ?
C13 C14 C15 127.1(14) . . ?
C13 C14 H14 116.4 . . ?
C15 C14 H14 116.4 . . ?
C14 C13 C12 134.1(13) . . ?
C14 C13 H13 112.9 . . ?
C12 C13 H13 112.9 . . ?
C6 C5 C4 127.1(13) . . ?
C6 C5 H5 116.5 . . ?
C4 C5 H5 116.5 . . ?
C16 C15 C14 127.6(15) . . ?
C16 C15 H15 116.2 . . ?
C14 C15 H15 116.2 . . ?
O9 C9 H92 109.5 . . ?
O9 C9 H93 109.5 . . ?
H92 C9 H93 109.5 . . ?
O9 C9 H91 109.5 . . ?
H92 C9 H91 109.5 . . ?
H93 C9 H91 109.5 . . ?
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 O2 2.317(9) . ?
Pb1 O1 2.346(9) . ?
Pb1 O9 2.559(10) . ?
Pb1 O11 2.597(8) . ?
Pb1 O3 2.672(9) . ?
Pb2 O12 2.350(9) . ?
Pb2 O11 2.361(9) . ?
Pb2 O6 2.569(11) . ?
O12 C12 1.302(14) . ?
O11 C11 1.280(13) . ?
O3 N1 1.237(13) . ?
O1 C1 1.307(14) . ?
O7 N2 1.226(15) . ?
N1 O5 1.211(13) . ?
N1 O4 1.254(13) . ?
O9 C9 1.375(18) . ?
O9 H9 0.9300 . ?
C11 C17 1.411(16) . ?
C11 C12 1.470(16) . ?
O6 N2 1.243(15) . ?
C12 C13 1.379(17) . ?
N2 O8 1.229(16) . ?
C17 C16 1.39(2) . ?
C17 H17 0.9300 . ?
C1 C7 1.394(17) . ?
C1 C2 1.479(15) . ?
C7 C6 1.380(19) . ?
C7 H7 0.9300 . ?
C16 C15 1.34(3) . ?
C16 H16 0.9300 . ?
C6 C5 1.34(2) . ?
C6 H6 0.9300 . ?
O2 C2 1.277(14) . ?
C3 C4 1.37(2) . ?
C3 C2 1.403(16) . ?
C3 H3 0.9300 . ?
C4 C5 1.41(2) . ?
C4 H4 0.9300 . ?
C14 C13 1.37(2) . ?
C14 C15 1.37(2) . ?
C14 H14 0.9300 . ?
C13 H13 0.9300 . ?
C5 H5 0.9300 . ?
C15 H15 0.9300 . ?
C9 H92 0.9600 . ?
C9 H93 0.9600 . ?
C9 H91 0.9600 . ?
