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_4307060
_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 Cl O8 Pb1.5'
_chemical_formula_weight         652.46
_chemical_name_systematic
; 
catena-(tetrakis(\m~3~-Tropolonato-O,O,O',O')-(\m~3~-perchlorato-O,O',O'',O''')
(\m~2~-perchlorato-O,O',O'',O''')-tri-lead(II))

;
_space_group_IT_number           13
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yac'
_symmetry_space_group_name_H-M   'P 1 2/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                 101.72(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.030(2)
_cell_length_b                   9.0607(18)
_cell_length_c                   14.652(3)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      15
_cell_measurement_theta_min      6
_cell_volume                     1563.8(5)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.910
_diffrn_measurement_device_type  'KUMA KM-4 four circle diffractometer'
_diffrn_measurement_method       'profile data 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  0.0913
_diffrn_reflns_av_sigmaI/netI    0.0756
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            3906
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         28.80
_diffrn_reflns_theta_min         2.00
_diffrn_standards_decay_%        2.14
_diffrn_standards_interval_count 200
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    16.360
_exptl_absorpt_correction_T_max  0.09154
_exptl_absorpt_correction_T_min  0.02208
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
Oxford Diffraction CCD Data Reduction, ver. 1.169.8
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    2.771
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'rectangular blocks'
_exptl_crystal_F_000             1192
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.31
_exptl_crystal_size_min          0.22
_refine_diff_density_max         3.444
_refine_diff_density_min         -3.590
_refine_diff_density_rms         0.449
_refine_ls_extinction_coef       0.0052(4)
_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   1.009
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     224
_refine_ls_number_reflns         3731
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.009
_refine_ls_R_factor_all          0.1039
_refine_ls_R_factor_gt           0.0474
_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^)+(0.1111P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1252
_refine_ls_wR_factor_ref         0.1565
_reflns_number_gt                2382
_reflns_number_total             3731
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic061561f-file002_3.cif
_cod_data_source_block           Pbtrop2
_cod_original_cell_volume        1563.7(5)
_cod_original_sg_symbol_H-M      'P 2/n'
_cod_original_formula_sum        'C14 H10 Cl O8 Pb1.50'
_cod_database_code               4307060