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_4320659
_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
;
(Cd 2+), (Br -1)2, (C20 H31 N7 Cd Br2)2, (H2 O)3
;
_chemical_formula_sum            'C40 H68 Br6 Cd3 N14 O3'
_chemical_formula_weight         1609.74
_chemical_name_systematic
;
  ?
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/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                90.00
_cell_angle_beta                 117.37(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.504(9)
_cell_length_b                   21.9400(10)
_cell_length_c                   15.7260(10)
_cell_measurement_reflns_used    20
_cell_measurement_temperature    298
_cell_measurement_theta_max      10.0
_cell_measurement_theta_min      7.0
_cell_volume                     5363(4)
_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 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  0.1245
_diffrn_reflns_av_sigmaI/netI    0.3134
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            3426
_diffrn_reflns_theta_full        21.99
_diffrn_reflns_theta_max         21.99
_diffrn_reflns_theta_min         2.54
_diffrn_standards_interval_time  60
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    5.699
_exptl_absorpt_correction_T_max  0.57
_exptl_absorpt_correction_T_min  0.14
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.994
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             3136
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.978
_refine_diff_density_min         -1.587
_refine_diff_density_rms         0.299
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.987
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     181
_refine_ls_number_reflns         3279
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.987
_refine_ls_R_factor_all          0.2832
_refine_ls_R_factor_gt           0.0972
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1906P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2591
_refine_ls_wR_factor_ref         0.3473
_reflns_number_gt                1349
_reflns_number_total             3279
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic010597z_1.cif
_cod_data_source_block           '[CdBr2(CdLBr2)2].2H2O'
_cod_original_cell_volume        5363(3)
_cod_database_code               4320659