Synthesis and Structure of the First Chiral Tetracoordinated Aluminum Cation
Norbert Emig; Régis Réau; Harald Krautscheid; Dieter Fenske; Guy Bertrand; Journal of the American Chemical Society 118 (1996) 5822–5823; doi:10.1021/ja953700q

data_4117153
_publ_contact_author
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Dr. G. Bertrand
Laboratoire de Chimie de Coordination CNRS
205, route de Narbonne
F-31077 Toulouse Cedex
France
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_publ_contact_author_email       gbertran@lcctoul.lcc-toulouse.fr
_publ_contact_author_fax         '(33) 61553003'
_publ_contact_author_phone       '(33) 61333124'
_publ_section_title
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 Synthesis and Structure of the First Chiral Tetracoordinated Aluminum
 Cation
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_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              5822
_journal_page_last               5823
_journal_paper_doi               10.1021/ja953700q
_journal_volume                  118
_journal_year                    1996
_chemical_formula_analytical     'C13 H35 Al Cl N3 Si3'
_chemical_formula_moiety         'C13 H35 Al Cl N3 Si3'
_chemical_formula_structural     'C13 H35 Al Cl N3 Si3'
_chemical_formula_sum            'C13 H35 Al Cl N3 Si3'
_chemical_formula_weight         380.14
_chemical_melting_point          289
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 92.07(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.349(4)
_cell_length_b                   10.226(2)
_cell_length_c                   13.352(4)
_cell_measurement_reflns_used    47
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      12
_cell_measurement_theta_min      5
_cell_volume                     2230.8(10)
_computing_cell_refinement       'STADI IV (Stoe, Darmstadt)'
_computing_data_collection       'STADI IV (Stoe, Darmstadt)'
_computing_data_reduction        'XRED (Stoe, Darmstadt)'
_computing_molecular_graphics    'CRYSTALS User Guide (Watkin et al., 1985)'
_computing_publication_material  'SHELXL-92 (Sheldrick, 1993)'
_computing_structure_refinement  'SHELXL-92 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      200(2)
_diffrn_measurement_device       'STOE-Stadi IV'
_diffrn_measurement_method       omega-scan
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoKa
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0139
_diffrn_reflns_av_sigmaI/netI    0.0181
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            8072
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         2.35
_diffrn_standards_decay_%        2
_diffrn_standards_interval_time  '2 h'
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.371
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.132
_exptl_crystal_description       prisms
_exptl_crystal_F_000             824
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.45
_exptl_crystal_size_min          0.35
_refine_diff_density_max         .290
_refine_diff_density_min         -.251
_refine_diff_density_rms         .038
_refine_ls_extinction_coef       0.005(1)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^l^3^/sin(2q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_all   1.033
_refine_ls_goodness_of_fit_obs   1.071
_refine_ls_hydrogen_treatment    'placed in estimated positions'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     331
_refine_ls_number_reflns         4339
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.042
_refine_ls_restrained_S_obs      1.071
_refine_ls_R_factor_all          0.0360
_refine_ls_R_factor_obs          0.0292
_refine_ls_shift/esd_max         0.005
_refine_ls_shift/esd_mean        0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[s^2^(Fo^2^)+( 0.0447P)^2^+0.5943P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0830
_refine_ls_wR_factor_obs         0.0788
_reflns_number_observed          3777
_reflns_number_total             4375
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ja953700q_1.cif
_cod_data_source_block           '[C13H35AlClN3Si3]'
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc w=1/[s^2^(Fo^2^)+(
0.0447P)^2^+0.5943P] where P=(Fo^2^+2Fc^2^)/3' was changed to 'calc'.
New tag '_refine_ls_weighting_details' was created. The value of the
new tag was set to 'w=1/[s^2^(Fo^2^)+( 0.0447P)^2^+0.5943P] where
P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
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_cod_database_code               4117153