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_4307059
_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            'C8 H7 F3 O6 Pb S'
_chemical_formula_weight         495.39
_chemical_name_systematic
; 
catena-(Aqua-(\m~2~-trifluoromethanesulfonato-O,O')
(\m~3~-tropolonato-O,O,O',O')-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                84.92(3)
_cell_angle_beta                 77.81(3)
_cell_angle_gamma                87.29(3)
_cell_formula_units_Z            2
_cell_length_a                   7.6850(15)
_cell_length_b                   8.2317(16)
_cell_length_c                   9.959(2)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      15
_cell_measurement_theta_min      6
_cell_volume                     613.1(2)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'KUMA KM-4 four circles 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  0.0259
_diffrn_reflns_av_sigmaI/netI    0.0316
_diffrn_reflns_limit_h_max       0
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            3839
_diffrn_reflns_theta_full        30.13
_diffrn_reflns_theta_max         30.13
_diffrn_reflns_theta_min         2.10
_diffrn_standards_decay_%        0.30
_diffrn_standards_interval_count 200
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    13.987
_exptl_absorpt_correction_T_max  0.26427
_exptl_absorpt_correction_T_min  0.14123
_exptl_absorpt_correction_type   analytical
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    2.683
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'rectangular rods'
_exptl_crystal_F_000             456
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.09
_refine_diff_density_max         3.894
_refine_diff_density_min         -3.607
_refine_diff_density_rms         0.292
_refine_ls_extinction_coef       0.042(2)
_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   1.065
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     179
_refine_ls_number_reflns         3579
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.064
_refine_ls_R_factor_all          0.0550
_refine_ls_R_factor_gt           0.0403
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0854P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1046
_refine_ls_wR_factor_ref         0.1105
_reflns_number_gt                2949
_reflns_number_total             3579
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic061561f-file002_2.cif
_cod_data_source_block           Pbtrop1
_cod_database_code               4307059