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_4319860
_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 H31 N7, Zn, (Cl O4)2
;
_chemical_formula_sum            'C20 H31 Cl2 N7 O8 Zn'
_chemical_formula_weight         633.79
_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                90.00
_cell_angle_beta                 94.010(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.8480(10)
_cell_length_b                   11.2760(10)
_cell_length_c                   19.688(3)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    298
_cell_measurement_theta_max      20
_cell_measurement_theta_min      12
_cell_volume                     2623.8(5)
_computing_cell_refinement       'XSCANS, SIEMENS'
_computing_data_collection       'XSCANS, SIEMENS'
_computing_data_reduction        'XSCANS, SIEMENS'
_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 0.970
_diffrn_measured_fraction_theta_max 0.970
_diffrn_measurement_device_type  'SIEMENS P4'
_diffrn_measurement_method       \q/2\q
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54180
_diffrn_reflns_av_R_equivalents  0.0500
_diffrn_reflns_av_sigmaI/netI    0.0360
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -1
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -1
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            5406
_diffrn_reflns_theta_full        64.18
_diffrn_reflns_theta_max         64.18
_diffrn_reflns_theta_min         3.74
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 200
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    3.694
_exptl_absorpt_correction_T_max  0.38
_exptl_absorpt_correction_T_min  0.25
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.604
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             1312
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.3
_refine_diff_density_max         0.549
_refine_diff_density_min         -0.571
_refine_diff_density_rms         0.080
_refine_ls_extinction_coef       0.00079(17)
_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   1.053
_refine_ls_hydrogen_treatment    refU
_refine_ls_matrix_type           full
_refine_ls_number_parameters     389
_refine_ls_number_reflns         4239
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.0635
_refine_ls_R_factor_gt           0.0574
_refine_ls_shift/su_max          0.016
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1097P)^2^+2.2739P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1707
_refine_ls_wR_factor_ref         0.1772
_reflns_number_gt                3704
_reflns_number_total             4239
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic001381k_1.cif
_cod_data_source_block           '[ZnL2](ClO4)2'
_cod_database_code               4319860