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_4084465
_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_moiety         'C27 H63 Sc Si6'
_chemical_formula_sum            'C27 H63 Sc Si6'
_chemical_formula_weight         601.27
_chemical_name_common            hannr01
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           33
_space_group_name_Hall           'P 2c -2n'
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2c -2n'
_symmetry_space_group_name_H-M   'P n a 21'
_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                90.00
_cell_formula_units_Z            4
_cell_length_a                   20.353(4)
_cell_length_b                   10.3936(19)
_cell_length_c                   18.749(3)
_cell_measurement_reflns_used    4062
_cell_measurement_temperature    100.0(5)
_cell_measurement_theta_max      18.65
_cell_measurement_theta_min      2.20
_cell_volume                     3966.2(12)
_computing_cell_refinement       'SAINT (Bruker, 2009)'
_computing_data_collection       'APEX2 (Bruker, 2012)'
_computing_data_reduction        'SAINT (Bruker, 2009)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR97 (Altomare et al., 1999)'
_diffrn_ambient_temperature      100.0(5)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker SMART APEX II CCD Platform'
_diffrn_measurement_method       '\w 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  0.1035
_diffrn_reflns_av_sigmaI/netI    0.0623
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            47647
_diffrn_reflns_theta_full        25.03
_diffrn_reflns_theta_max         25.03
_diffrn_reflns_theta_min         2.00
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.380
_exptl_absorpt_correction_T_max  0.9417
_exptl_absorpt_correction_T_min  0.8690
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2008)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.007
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1320
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.870
_refine_diff_density_min         -0.271
_refine_diff_density_rms         0.097
_refine_ls_abs_structure_details
'Flack H D (1983), 3390 Friedel pairs, Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.189
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     276
_refine_ls_number_reflns         7017
_refine_ls_number_restraints     979
_refine_ls_restrained_S_all      1.199
_refine_ls_R_factor_all          0.2251
_refine_ls_R_factor_gt           0.1306
_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^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3318
_refine_ls_wR_factor_ref         0.4041
_reflns_number_gt                2971
_reflns_number_total             7017
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om5009204_si_003.cif
_cod_data_source_block           hannr01
_cod_depositor_comments
'Adding full bibliography for 4084464--4084465.cif.'
_cod_database_code               4084465