Synthesis and Structural Characterization of Heterometallic Thorium Aluminum Polynuclear Molecular Clusters
Melissa Fairley; Daniel K. Unruh; Samangi Abeysinghe; Tori Z. Forbes; Inorganic Chemistry 51 (2012) 9491–9498; doi:10.1021/ic3013014

data_4330267
_publ_contact_author_address
;Department of Chemistry
W374 Chemistry Building
The University of Iowa
Iowa City, IA 52242-1294
USA
;
_publ_contact_author_fax         1-319-335-1270
_publ_contact_author_name        'Forbes, Tori M.'
_publ_contact_author_phone       1-319-384-1908
_publ_section_title
;
 Synthesis and Structural Characterization of Heterometallic Thorium
 Aluminum Polynuclear Molecular Clusters
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              9491
_journal_page_last               9498
_journal_paper_doi               10.1021/ic3013014
_journal_volume                  51
_journal_year                    2012
_chemical_formula_sum            'C20 H44 Al6 N10 O70 Th2'
_chemical_formula_weight         2170.61
_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_date             2011-10-10T16:06:40-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 96.375(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   11.1979(12)
_cell_length_b                   14.2103(16)
_cell_length_c                   23.115(3)
_cell_measurement_reflns_used    9829
_cell_measurement_temperature    210(2)
_cell_measurement_theta_max      33.64
_cell_measurement_theta_min      2.8
_cell_volume                     3655.4(7)
_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      210(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'CCD phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.032
_diffrn_reflns_av_unetI/netI     0.0239
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            86956
_diffrn_reflns_theta_full        33.64
_diffrn_reflns_theta_max         33.64
_diffrn_reflns_theta_min         3.02
_exptl_absorpt_coefficient_mu    4.273
_exptl_absorpt_correction_T_max  0.7262
_exptl_absorpt_correction_T_min  0.5135
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.957
_exptl_crystal_description       blocky
_exptl_crystal_F_000             2104.0
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.08
_refine_diff_density_max         2.183
_refine_diff_density_min         -1.188
_refine_diff_density_rms         0.155
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.103
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     509
_refine_ls_number_reflns         14441
_refine_ls_number_restraints     8
_refine_ls_restrained_S_all      1.103
_refine_ls_R_factor_all          0.0406
_refine_ls_R_factor_gt           0.0311
_refine_ls_shift/su_max          0
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0369P)^2^+10.8518P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0796
_refine_ls_wR_factor_ref         0.0838
_reflns_number_gt                12436
_reflns_number_total             14441
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic3013014_si_001.cif
_cod_data_source_block           1
_cod_database_code               4330267