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_4117154
_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
;
 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 H36 Al Cl N3 Si3][Al Cl4]'
_chemical_formula_moiety         '[C13 H36 Al Cl N3 Si3][Al Cl4]'
_chemical_formula_structural     '[C13 H36 Al Cl N3 Si3][Al Cl4]'
_chemical_formula_sum            'C13 H36 Al2 Cl5 N3 Si3'
_chemical_formula_weight         549.93
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                82.62(3)
_cell_angle_beta                 68.94(3)
_cell_angle_gamma                89.17(3)
_cell_formula_units_Z            2
_cell_length_a                   9.992(4)
_cell_length_b                   11.970(4)
_cell_length_c                   13.160(5)
_cell_measurement_reflns_used    32
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      12
_cell_measurement_theta_min      5
_cell_volume                     1455.8(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  0.0125
_diffrn_reflns_av_sigmaI/netI    0.0269
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            4567
_diffrn_reflns_theta_max         24.00
_diffrn_reflns_theta_min         1.67
_diffrn_standards_decay_%        3
_diffrn_standards_interval_time  '1 h'
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.688
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.255
_exptl_crystal_description       prisms
_exptl_crystal_F_000             576
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.25
_refine_diff_density_max         .535
_refine_diff_density_min         -.444
_refine_diff_density_rms         .051
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.034
_refine_ls_goodness_of_fit_obs   1.060
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     248
_refine_ls_number_reflns         4265
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.037
_refine_ls_restrained_S_obs      1.060
_refine_ls_R_factor_all          0.0559
_refine_ls_R_factor_obs          0.0374
_refine_ls_shift/esd_max         0.012
_refine_ls_shift/esd_mean        0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[s^2^(Fo^2^)+( 0.0437P)^2^+1.4439P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1026
_refine_ls_wR_factor_obs         0.0916
_reflns_number_observed          3312
_reflns_number_total             4267
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ja953700q_2.cif
_cod_data_source_block           '[C13H36Al2Cl5N3Si3]'
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc w=1/[s^2^(Fo^2^)+(
0.0437P)^2^+1.4439P] 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^)+( 0.0437P)^2^+1.4439P] where
P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        1455.8(9)
_cod_database_code               4117154