A Seven-Membered Aluminum Sulfur Allenyl Heterocycle Arising from the Conversion of an Aluminacyclopropene with CS2
Hongping Zhu; Jianfang Chai; Qingjun Ma; Vojtech Jancik; Herbert W. Roesky; Hongjun Fan; Regine Herbst-Irmer; Journal of the American Chemical Society 126 (2004) 10194–10195; doi:10.1021/ja049462t

data_4112886
_publ_section_title
;
 A Seven-Membered Aluminum Sulfur Allenyl Heterocycle Arising from the
 Conversion of an Aluminacyclopropene with CS2
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              10194
_journal_page_last               10195
_journal_paper_doi               10.1021/ja049462t
_journal_volume                  126
_journal_year                    2004
_chemical_formula_sum            'C42.32 H68.79 Al N2 O2.89 Si2'
_chemical_formula_weight         735.10
_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-97
_cell_angle_alpha                77.19(3)
_cell_angle_beta                 87.82(3)
_cell_angle_gamma                81.06(3)
_cell_formula_units_Z            2
_cell_length_a                   10.166(2)
_cell_length_b                   12.781(3)
_cell_length_c                   17.393(4)
_cell_measurement_reflns_used    6840
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      58.926
_cell_measurement_theta_min      6.820
_cell_volume                     2176.9(9)
_computing_cell_refinement       'Siemens SAINT (V6.31a,Siemens 2002)'
_computing_data_collection       'Proteum (Version 1.35)'
_computing_data_reduction        'Siemens SAINT (V6.31a,Siemens 2002)'
_computing_molecular_graphics    'Bruker AXS SHELXTL (V5.10)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.973
_diffrn_measured_fraction_theta_max 0.973
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0198
_diffrn_reflns_av_sigmaI/netI    0.0246
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            9795
_diffrn_reflns_theta_full        58.94
_diffrn_reflns_theta_max         58.94
_diffrn_reflns_theta_min         4.88
_exptl_absorpt_coefficient_mu    1.216
_exptl_absorpt_correction_T_max  0.8881
_exptl_absorpt_correction_T_min  0.8881
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.121
_exptl_crystal_description       block
_exptl_crystal_F_000             802
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.419
_refine_diff_density_min         -0.333
_refine_diff_density_rms         0.043
_refine_ls_extinction_coef       0.0042(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    'riding model'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     534
_refine_ls_number_reflns         6103
_refine_ls_number_restraints     213
_refine_ls_restrained_S_all      1.017
_refine_ls_R_factor_all          0.0368
_refine_ls_R_factor_gt           0.0357
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0401P)^2^+1.5570P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0885
_refine_ls_wR_factor_ref         0.0895
_reflns_number_gt                5857
_reflns_number_total             6103
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja049462tsi20040727_101431.cif
_cod_data_source_block           compound3
_cod_original_cell_volume        2176.9(8)
_cod_database_code               4112886