Eight-Coordinate Zn(II), Cd(II), and Pb(II) Complexes Based on a 1,7-Diaza-12-crown-4 Platform Endowed with a Remarkable Selectivity over Ca(II)
Raquel Ferreirós-Martínez; David Esteban-Gómez; Andrés de Blas; Carlos Platas-Iglesias; Teresa Rodríguez-Blas; Inorganic Chemistry 48 (2009) 11821–11831; doi:10.1021/ic901883h

data_4303911
_publ_contact_author_address
;
Departamento de Quimica Fundamental
Facultade de Ciencias
Universidade da Coruna
Campus da Zapateira s/n
15071 A Coruna
Spain
;
_publ_contact_author_email       ucambv@udc.es
_publ_contact_author_fax         '+ 34 981 167065'
_publ_contact_author_name        'De Blas, Andres'
_publ_contact_author_phone       '+ 34 981 167000'
_publ_section_title
;
Eight-Coordinate Zn(II), Cd(II), and Pb(II) Complexes Based on a
1,7-Diaza-12-crown-4 Platform Endowed with a Remarkable Selectivity over
Ca(II)
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              11821
_journal_page_last               11831
_journal_paper_doi               10.1021/ic901883h
_journal_volume                  48
_journal_year                    2009
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety
'2(C22 H27 N4 O6 Zn), C H4 O, 2(Cl O4), 5(H2 O)'
_chemical_formula_sum            'C45 H68 Cl2 N8 O26 Zn2'
_chemical_formula_weight         1338.71
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_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_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.4
_audit_creation_date             2009-03-19T10:57:36-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 93.658(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.5316(16)
_cell_length_b                   28.823(4)
_cell_length_c                   15.644(2)
_cell_measurement_reflns_used    7842
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.9686
_cell_measurement_theta_min      4.4658
_cell_measurement_wavelength     0.71073
_cell_volume                     5639.1(13)
_computing_cell_refinement
'SAINT V7.12A (Bruker Nonius 2004) in Apex2 suite.'
_computing_data_collection       'Apex2  V.1.0-27 (Bruker Nonius, 2005);'
_computing_data_reduction
'SAINT and XPREP Version 6.14 COPYRIGHT(c) 2003 Bruker-AXS'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    DIRDIF99
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Bruker X8 APEXII CCD'
_diffrn_measurement_method       'omega and  phi rotation with narrow frames'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0576
_diffrn_reflns_av_unetI/netI     0.0569
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       38
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            54810
_diffrn_reflns_theta_full        28.38
_diffrn_reflns_theta_max         28.38
_diffrn_reflns_theta_min         2.57
_exptl_absorpt_coefficient_mu    1.038
_exptl_absorpt_correction_T_max  0.969
_exptl_absorpt_correction_T_min  0.774
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS. Bruker AXS Inc., Madison,
Wisconsin, USA. or Sheldrick, G. M. (1996). 
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.577
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2784
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.327
_refine_diff_density_min         -0.637
_refine_diff_density_rms         0.093
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.019
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     797
_refine_ls_number_reflns         14009
_refine_ls_number_restraints     15
_refine_ls_restrained_S_all      1.019
_refine_ls_R_factor_all          0.0752
_refine_ls_R_factor_gt           0.0455
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0517P)^2^+3.9748P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1034
_refine_ls_wR_factor_ref         0.1158
_reflns_number_gt                10044
_reflns_number_total             14009
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            ic901883h_si_002_5.cif
_cod_data_source_block           compound3c
_cod_original_cell_volume        5639.2(13)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4303911