Protonation and Zn(II) Coordination by Dipyridine-Containing Macrocycles with Different Molecular Architecture. A Case of pH-Controlled Metal Jumping Outside-Inside the Macrocyclic Cavity
Carlos Lodeiro; A. Jorge Parola; Fernando Pina; Carla Bazzicalupi; Andrea Bencini; Antonio Bianchi; Claudia Giorgi; Andrea Masotti; Barbara Valtancoli; Inorganic Chemistry 40 (2001) 2968–2975; doi:10.1021/ic001381k

data_4319861
_publ_section_title
;
 Protonation and Zn(II) Coordination by Dipyridine-Containing Macrocycles
 with Different Molecular Architecture. A Case of pH-Controlled Metal
 Jumping Outside-Inside the Macrocyclic Cavity
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2968
_journal_page_last               2975
_journal_paper_doi               10.1021/ic001381k
_journal_volume                  40
_journal_year                    2001
_chemical_formula_moiety
;
C20 H35 N7, (Cl O4)4, H2 O
;
_chemical_formula_sum            'C20 H37 Cl4 N7 O17'
_chemical_formula_weight         789.37
_chemical_name_systematic
;
 ?
;
_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                91.17(3)
_cell_angle_beta                 97.12(5)
_cell_angle_gamma                94.23(5)
_cell_formula_units_Z            2
_cell_length_a                   8.758(9)
_cell_length_b                   9.662(3)
_cell_length_c                   19.190(7)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    298
_cell_measurement_theta_max      13
_cell_measurement_theta_min      7
_cell_volume                     1606.2(18)
_computing_cell_refinement       'ENRAF NONIUS CAD4'
_computing_data_collection       'ENRAF NONIUS CAD4'
_computing_data_reduction        'ENRAF NONIUS CAD4'
_computing_molecular_graphics    'ORTEP3 Ver. 1.01\b (Farrugia, 1997)'
_computing_publication_material  'PARST93 (Nardelli, 1993)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR97 (Altomare, 1997)'
_diffrn_ambient_temperature      298
_diffrn_measured_fraction_theta_full 0.814
_diffrn_measured_fraction_theta_max 0.814
_diffrn_measurement_device_type  'ENRAF NONUIS 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  0.0332
_diffrn_reflns_av_sigmaI/netI    0.0830
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            4721
_diffrn_reflns_theta_full        24.97
_diffrn_reflns_theta_max         24.97
_diffrn_reflns_theta_min         2.70
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  60
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    0.455
_exptl_absorpt_correction_T_max  0.95
_exptl_absorpt_correction_T_min  0.85
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.632
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prosmatic
_exptl_crystal_F_000             820
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.868
_refine_diff_density_min         -0.353
_refine_diff_density_rms         0.081
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     470
_refine_ls_number_reflns         4586
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.1056
_refine_ls_R_factor_gt           0.0672
_refine_ls_shift/su_max          0.056
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1056P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1795
_refine_ls_wR_factor_ref         0.1957
_reflns_number_gt                3184
_reflns_number_total             4586
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic001381k_2.cif
_cod_data_source_block           '[H4L3](ClO4)4.H2O'
_cod_database_code               4319861