Synthesis and Characterization of an Al693- Cluster with 51 Naked Al Atoms: Analogies and Differences to the Previously Characterized Al772- Cluster
Harald Köhnlein; Andreas Purath; Christoph Klemp; Elke Baum; Ingo Krossing; Gregor Stösser; Hansgeorg Schnöckel; Inorganic Chemistry 40 (2001) 4830–4838; doi:10.1021/ic0104297

data_4320257
_publ_contact_author
;
    Prof. Dr. H: Schn\"ockel
    Inst. f. Anorganische
    der Universit\"at Karlsruhe (TH)
    Engesserstr. Geb. 30.45
    76128 Karlsruhe
    GERMANY
;
_publ_contact_author_email       hg@achpc9.chemie.uni-karlsruhe.de
_publ_contact_author_fax         '(49) 721 608 4854'
_publ_contact_author_phone       '(49) 721 608 2980'
_publ_section_title
;
 Synthesis and Characterization of an Al693- Cluster with 51 Naked Al
 Atoms: Analogies and Differences to the Previously Characterized Al772-
 Cluster
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4830
_journal_page_last               4838
_journal_paper_doi               10.1021/ic0104297
_journal_volume                  40
_journal_year                    2001
_chemical_formula_sum            'C150 H372 Al69 Li3 N18 O12 Si36'
_chemical_formula_weight         5514.34
_chemical_name_systematic
;
   ?
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/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                 96.11(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   29.172(6)
_cell_length_b                   37.665(8)
_cell_length_c                   31.502(6)
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      22.50
_cell_measurement_theta_min      2.07
_cell_volume                     34417(12)
_computing_data_collection       'Nonius software'
_computing_data_reduction        'Nonius software'
_computing_molecular_graphics    'Diamond 2.1'
_computing_publication_material  SHELX
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'NONIUS KAPPA CCD'
_diffrn_measurement_method       CCD
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0828
_diffrn_reflns_av_sigmaI/netI    0.1931
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       40
_diffrn_reflns_limit_k_min       -38
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            43008
_diffrn_reflns_theta_full        22.50
_diffrn_reflns_theta_max         22.50
_diffrn_reflns_theta_min         2.07
_exptl_absorpt_coefficient_mu    0.345
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.064
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             11616
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.610
_refine_diff_density_min         -0.686
_refine_diff_density_rms         0.145
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.204
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1092
_refine_ls_number_reflns         22466
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.204
_refine_ls_R_factor_all          0.2523
_refine_ls_R_factor_gt           0.1296
_refine_ls_shift/su_max          0.082
_refine_ls_shift/su_mean         0.010
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3705
_refine_ls_wR_factor_ref         0.4279
_reflns_number_gt                8787
_reflns_number_total             22466
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0104297_1.cif
_cod_data_source_block           hk34mo
_cod_database_code               4320257