Tris(pyrazolyl)borate Complexes of the Alkaline-Earth Metals: Alkylaluminate Precursors and Schlenk-Type Rearrangements
Michel, Olaf; Dietrich, H. Martin; Litlabø, Rannveig; Törnroos, Karl W.; Maichle-Mössmer, Cäcilia; Anwander, Reiner; Organometallics 31 (2012) 3119–; doi:10.1021/om300032c

data_4078009
_publ_section_title
;
 Tris(pyrazolyl)borate Complexes of the Alkaline-Earth Metals:
 Alkylaluminate Precursors and Schlenk-Type Rearrangements
;
_journal_issue                   8
_journal_name_full               Organometallics
_journal_page_first              3119
_journal_paper_doi               10.1021/om300032c
_journal_volume                  31
_journal_year                    2012
_chemical_formula_moiety         'C24 H60 Al3 Ba K'
_chemical_formula_sum            'C24 H60 Al3 Ba K'
_chemical_formula_weight         606.10
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           148
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  '-R 3'
_symmetry_space_group_name_H-M   'R -3 :H'
_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                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            6
_cell_length_a                   13.1949(8)
_cell_length_b                   13.1949(8)
_cell_length_c                   32.321(3)
_cell_measurement_temperature    173(2)
_cell_volume                     4873.4(6)
_computing_cell_refinement       X-AREA
_computing_data_collection       X-AREA
_computing_data_reduction        X-AREA
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device_type  'STOE IPDS II'
_diffrn_measurement_method       omega-scans
_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  0.0631
_diffrn_reflns_av_sigmaI/netI    0.0210
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       44
_diffrn_reflns_limit_l_min       -44
_diffrn_reflns_number            30403
_diffrn_reflns_theta_full        29.07
_diffrn_reflns_theta_max         29.07
_diffrn_reflns_theta_min         4.76
_exptl_absorpt_coefficient_mu    1.441
_exptl_absorpt_correction_T_max  0.83426
_exptl_absorpt_correction_T_min  0.45608
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   mulabs
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.239
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1908
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.40
_refine_diff_density_max         2.962
_refine_diff_density_min         -1.057
_refine_diff_density_rms         0.128
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.190
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     93
_refine_ls_number_reflns         2878
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.189
_refine_ls_R_factor_all          0.0411
_refine_ls_R_factor_gt           0.0394
_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^)+(0.0427P)^2^+41.8626P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1033
_refine_ls_wR_factor_ref         0.1041
_reflns_number_gt                2796
_reflns_number_total             2878
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om300032c_si_001.cif
_cod_data_source_block           Compound6
_cod_original_cell_volume        4873.3(6)
_cod_original_sg_symbol_H-M      R-3
_cod_database_code               4078009