Synthesis and characterization of homo- and heteronuclear molecular Al3+ and Th4+ species chelated by the ethylenediaminetetraacetate (edta) ligand.
Fairley, Melissa; Unruh, Daniel K.; Donovan, Amy; Abeysinghe, Samangi; Forbes, Tori Z.; Dalton transactions (Cambridge, England : 2003) 42 (2013) 13706–13714; doi:10.1039/c3dt51517f

data_7023584
_publ_section_title
;
 Synthesis and characterization of homo- and heteronuclear molecular Al3+
 and Th4+ species chelated by the ethylenediaminetetraacetate (edta)
 ligand.
;
_journal_issue                   37
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              13706
_journal_page_last               13714
_journal_paper_doi               10.1039/c3dt51517f
_journal_volume                  42
_journal_year                    2013
_chemical_formula_moiety
'[Th4(H2O)4Al10(H2O)8(OH)28(C10H12N2O8)4]?(H2O)32 '
_chemical_formula_sum            'C40 H48 Al10 N8 O103.5 Th4'
_chemical_formula_weight         3494.82
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_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                102.314(3)
_cell_angle_beta                 95.615(3)
_cell_angle_gamma                92.473(3)
_cell_formula_units_Z            1
_cell_length_a                   9.3172(8)
_cell_length_b                   16.6099(14)
_cell_length_c                   19.5080(14)
_cell_measurement_reflns_used    9844
_cell_measurement_temperature    483(2)
_cell_measurement_theta_max      26.20
_cell_measurement_theta_min      2.46
_cell_volume                     2929.0(4)
_computing_cell_refinement       'APEX2 (Bruker AXS, 2006)'
_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_data_reduction        'APEX2 (Bruker AXS, 2006)'
_computing_molecular_graphics    'CrystalMaker v2.5.0'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      483(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0451
_diffrn_reflns_av_sigmaI/netI    0.0342
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            70550
_diffrn_reflns_theta_full        26.37
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         2.55
_diffrn_source                   'fine-focus sealed tube'
_diffrn_source_type              'Nonius Kappa CCD'
_exptl_absorpt_coefficient_mu    5.268
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6469
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            clear
_exptl_crystal_density_diffrn    1.981
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       blocky
_exptl_crystal_F_000             1662
_exptl_crystal_size_max          0.080
_exptl_crystal_size_mid          0.030
_exptl_crystal_size_min          0.010
_refine_diff_density_max         2.162
_refine_diff_density_min         -1.171
_refine_diff_density_rms         0.185
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.079
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     693
_refine_ls_number_reflns         11946
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.079
_refine_ls_R_factor_all          0.0520
_refine_ls_R_factor_gt           0.0381
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0473P)^2^+22.2448P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0992
_refine_ls_wR_factor_ref         0.1062
_reflns_number_gt                9744
_reflns_number_total             11946
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3dt51517f.txt
_cod_data_source_block           p-1
_cod_depositor_comments
;
 Marking attached hydrogen atoms.

 Antanas Vaitkus,
 2016-12-21
;
_cod_original_formula_sum        'C40 H48 Al10 N8 O103.50 Th4'
_cod_database_code               7023584