Mechanochemical Synthesis of [1,3-(SiMe3)2C3H3]3(Al,Sc), a Base-Free Tris(allyl)aluminum Complex and Its Scandium Analogue
Rightmire, Nicholas R.; Hanusa, Timothy P.; Rheingold, Arnold L.; Organometallics 33 (2014) 5952–; doi:10.1021/om5009204

data_4084464
_publ_section_title
;
 Mechanochemical Synthesis of [1,3-(SiMe3)2C3H3]3(Al,Sc), a Base-Free
 Tris(allyl)aluminum Complex and Its Scandium Analogue
;
_journal_issue                   21
_journal_name_full               Organometallics
_journal_page_first              5952
_journal_paper_doi               10.1021/om5009204
_journal_volume                  33
_journal_year                    2014
_chemical_formula_sum            'C27 H63 Al Si6'
_chemical_formula_weight         583.29
_chemical_name_systematic
; 
 ? 
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                76.9090(14)
_cell_angle_beta                 87.3960(15)
_cell_angle_gamma                81.8680(15)
_cell_formula_units_Z            2
_cell_length_a                   10.2630(4)
_cell_length_b                   12.7306(5)
_cell_length_c                   15.8391(6)
_cell_measurement_reflns_used    4116
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.25
_cell_measurement_theta_min      2.34
_cell_volume                     1995.20(13)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.951
_diffrn_measured_fraction_theta_max 0.917
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0197
_diffrn_reflns_av_unetI/netI     0.0509
_diffrn_reflns_Laue_measured_fraction_full 0.951
_diffrn_reflns_Laue_measured_fraction_max 0.917
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            12686
_diffrn_reflns_point_group_measured_fraction_full 0.951
_diffrn_reflns_point_group_measured_fraction_max 0.917
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         28.304
_diffrn_reflns_theta_min         2.005
_exptl_absorpt_coefficient_mu    0.244
_exptl_absorpt_correction_T_max  0.955
_exptl_absorpt_correction_T_min  0.888
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    0.971
_exptl_crystal_description       plate
_exptl_crystal_F_000             644
_exptl_crystal_size_max          0.290
_exptl_crystal_size_mid          0.240
_exptl_crystal_size_min          0.100
_refine_diff_density_max         0.791
_refine_diff_density_min         -0.297
_refine_diff_density_rms         0.060
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.014
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     325
_refine_ls_number_reflns         9092
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.014
_refine_ls_R_factor_all          0.0657
_refine_ls_R_factor_gt           0.0438
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0540P)^2^+0.4000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1004
_refine_ls_wR_factor_ref         0.1115
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6906
_reflns_number_total             9092
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om5009204_si_003.cif
_cod_data_source_block           vand92
_cod_depositor_comments
'Adding full bibliography for 4084464--4084465.cif.'
_cod_database_code               4084464
_shelx_estimated_absorpt_t_min   0.932
_shelx_estimated_absorpt_t_max   0.976