Cd(II) and Pb(II) Complexation by Dipyridine-Containing Macrocycles with Different Molecular Architecture. Effect of Complex Protonation on Metal Coordination Environment
Paloma Arranz; Carla Bazzicalupi; Andrea Bencini; Antonio Bianchi; Samuele Ciattini; Patrizia Fornasari; Claudia Giorgi; Barbara Valtancoli; Inorganic Chemistry 40 (2001) 6383–6389; doi:10.1021/ic010597z

data_4320660
_publ_section_title
;
 Cd(II) and Pb(II) Complexation by Dipyridine-Containing Macrocycles with
 Different Molecular Architecture. Effect of Complex Protonation on Metal
 Coordination Environment
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6383
_journal_page_last               6389
_journal_paper_doi               10.1021/ic010597z
_journal_volume                  40
_journal_year                    2001
_chemical_formula_moiety
;
(C20 H31 N7 Pb 2+), (B C24 H20)2
;
_chemical_formula_sum            'C71 H77 B2 N7 Pb'
_chemical_formula_weight         1257.21
_chemical_name_systematic
;
  ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.000(5)
_cell_angle_beta                 106.430(5)
_cell_angle_gamma                90.000(5)
_cell_formula_units_Z            4
_cell_length_a                   11.335(5)
_cell_length_b                   28.526(5)
_cell_length_c                   19.635(5)
_cell_measurement_reflns_used    21
_cell_measurement_temperature    298
_cell_measurement_theta_max      12
_cell_measurement_theta_min      8
_cell_volume                     6090(3)
_computing_cell_refinement       'ENRAF NONIUS CAD4'
_computing_data_collection       'ENRAF NONIUS CAD4'
_computing_data_reduction        'ENRAF NONIUS CAD4'
_computing_molecular_graphics    'ORTEP-3 (Ver. 1.01\b) (Farrugia, 1997)'
_computing_publication_material  'PARST97 (Nardelli, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR97 (Altomare, 1999)'
_diffrn_ambient_temperature      298
_diffrn_measured_fraction_theta_full 0.804
_diffrn_measured_fraction_theta_max 0.804
_diffrn_measurement_device_type  'ENRAF NONIUS CAD4'
_diffrn_measurement_method       \q/2\q
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0797
_diffrn_reflns_av_sigmaI/netI    0.0742
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            8859
_diffrn_reflns_theta_full        24.98
_diffrn_reflns_theta_max         24.98
_diffrn_reflns_theta_min         2.52
_diffrn_standards_interval_time  60
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    2.819
_exptl_absorpt_correction_T_max  0.57
_exptl_absorpt_correction_T_min  0.49
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.371
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             2576
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.153
_refine_diff_density_min         -1.654
_refine_diff_density_rms         0.155
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    refU
_refine_ls_matrix_type           full
_refine_ls_number_parameters     734
_refine_ls_number_reflns         8617
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.0912
_refine_ls_R_factor_gt           0.0545
_refine_ls_shift/su_max          0.012
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0514P)^2^+48.5898P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1197
_refine_ls_wR_factor_ref         0.1475
_reflns_number_gt                6970
_reflns_number_total             8617
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic010597z_2.cif
_cod_data_source_block           '[PbL](BPh4)2'
_cod_database_code               4320660