Influence of pH and Counteranion on the Structure of Tropolonato-Lead(II) Complexes: Structural and Infrared Characterization of Formed Lead Compounds
Krzysztof Lyczko; Wojciech Starosta; Ingmar Persson; Inorganic Chemistry 46 (2007) 4402–4410; doi:10.1021/ic061561f

data_4307061
_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-((\m~3~Tropolonato-O,O,O',O')-(\m~2~-tropolonato-O,O,O')
(\m~2~-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 \w/2\q 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+0.001xFc^2^\l^3^/sin(2\q)]^-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/[\s^2^(Fo^2^)+(0.1213P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/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