Lightest Member of the Basic Carboxylate Structural Pattern: [Al3(μ3-O)(μ-O2CCF3)6(THF)3][(Me3Si)3CAl(O2CCF3)3].C7H8
Hagen Hatop; Marilena Ferbinteanu; Herbert W. Roesky; Fanica Cimpoesu; Marcus Schiefer; Hans-Georg Schmidt; Mathias Noltemeyer; Inorganic Chemistry 41 (2002) 1022–1025; doi:10.1021/ic010880y

data_4317573
_publ_contact_author
;
       Herbert W. Roesky
       Institut f\"ur Anorganische Chemie
       Universit\"at G\"ottingen
       Tammannstr. 4
       37077 G\"ottingen
       Germany;
;
_publ_contact_author_email       hroesky@gwdg.de
_publ_contact_author_fax         '049 551 393373'
_publ_contact_author_phone       '049 551 393001'
_publ_section_title
;
 Lightest Member of the Basic Carboxylate Structural Pattern:
 [Al3(\m3-O)(\m-O2CCF3)6(THF)3][(Me3Si)3CAl(O2CCF3)3].C7H8
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1022
_journal_page_last               1025
_journal_paper_doi               10.1021/ic010880y
_journal_volume                  41
_journal_year                    2002
_chemical_formula_sum            'C47 H59 Al4 F27 O22 Si3'
_chemical_formula_weight         1681.13
_chemical_name_systematic
;
    compound 1
;
_space_group_IT_number           148
_symmetry_cell_setting           rhombohedral
_symmetry_space_group_name_Hall  '-P 3*'
_symmetry_space_group_name_H-M   'R -3 :R'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                53.472(17)
_cell_angle_beta                 53.472(17)
_cell_angle_gamma                53.472(17)
_cell_formula_units_Z            2
_cell_length_a                   18.313(2)
_cell_length_b                   18.313(2)
_cell_length_c                   18.313(2)
_cell_measurement_reflns_used    38
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      12.5
_cell_measurement_theta_min      10
_cell_volume                     3679.3(12)
_computing_cell_refinement       DIF4
_computing_data_collection       DIF4
_computing_data_reduction        REDU4
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      200(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'STOE AED2'
_diffrn_measurement_method       'profile fit'
_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  0.1241
_diffrn_reflns_av_sigmaI/netI    0.0268
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            4633
_diffrn_reflns_theta_full        25.05
_diffrn_reflns_theta_max         25.05
_diffrn_reflns_theta_min         3.59
_diffrn_standards_decay_%        none
_diffrn_standards_interval_time  '90 min'
_exptl_absorpt_coefficient_mu    0.246
_exptl_absorpt_correction_T_max  0.8868
_exptl_absorpt_correction_T_min  0.7909
_exptl_crystal_colour            none
_exptl_crystal_density_diffrn    1.517
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       blocks
_exptl_crystal_F_000             1708
_exptl_crystal_size_max          1.00
_exptl_crystal_size_mid          0.70
_exptl_crystal_size_min          0.50
_refine_diff_density_max         1.284
_refine_diff_density_min         -0.698
_refine_diff_density_rms         0.080
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.013
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     368
_refine_ls_number_reflns         4341
_refine_ls_number_restraints     599
_refine_ls_restrained_S_all      0.971
_refine_ls_R_factor_all          0.0889
_refine_ls_R_factor_gt           0.0712
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1120P)^2^+7.9020P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1918
_refine_ls_wR_factor_ref         0.2112
_reflns_number_gt                3445
_reflns_number_total             4341
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic010880y.cif
_cod_data_source_block           roe934x
_cod_original_cell_volume        3679.3(7)
_cod_original_sg_symbol_H-M      'R -3'
_cod_database_code               4317573