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_4303908
_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_absolute_configuration ad
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C22 H26 N4 O6 Pb, 2(C6 H16 N), 2(Cl O4)'
_chemical_formula_sum            'C34 H58 Cl2 N6 O14 Pb'
_chemical_formula_weight         1052.95
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           29
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      29
_symmetry_space_group_name_Hall  'P 2c -2ac'
_symmetry_space_group_name_H-M   'P c a 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     heavy
_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             2009-03-20T12:03:16-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.3662(6)
_cell_length_b                   22.5993(12)
_cell_length_c                   15.0562(8)
_cell_measurement_reflns_used    1947
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      22.31
_cell_measurement_theta_min      2.315
_cell_measurement_wavelength     0.71073
_cell_volume                     4207.7(4)
_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 (Beurskens et al, 1999)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker X8 APEXII CCD'
_diffrn_measurement_method       'omega and  phi scans'
_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  0.0682
_diffrn_reflns_av_unetI/netI     0.0838
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            8614
_diffrn_reflns_theta_full        26.4
_diffrn_reflns_theta_max         26.4
_diffrn_reflns_theta_min         0.9
_exptl_absorpt_coefficient_mu    4.207
_exptl_absorpt_correction_T_max  0.881
_exptl_absorpt_correction_T_min  0.563
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SABADS, Bruker-AXS  Version 2004/1
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.662
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2128
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.508
_refine_diff_density_min         -1.304
_refine_diff_density_rms         0.138
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.502(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     541
_refine_ls_number_reflns         8614
_refine_ls_number_restraints     241
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.0931
_refine_ls_R_factor_gt           0.0494
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0402P)^2^+15.7164P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0973
_refine_ls_wR_factor_ref         0.1131
_reflns_number_gt                6017
_reflns_number_total             8614
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            ic901883h_si_002_2.cif
_cod_data_source_block           compound1b
_cod_database_code               4303908