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_4112885
_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            'C72.65 H108.9 Al2 N4 O0.45 S2 Si2'
_chemical_formula_weight         1219.82
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           9
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'C -2yc'
_symmetry_space_group_name_H-M   'C 1 c 1'
_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                 94.36(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   18.903(4)
_cell_length_b                   18.624(4)
_cell_length_c                   20.125(4)
_cell_measurement_reflns_used    3878
_cell_measurement_temperature    133(2)
_cell_measurement_theta_max      60.203
_cell_measurement_theta_min      6.684
_cell_volume                     7064(3)
_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      133(2)
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_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  0.0347
_diffrn_reflns_av_sigmaI/netI    0.0573
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            15563
_diffrn_reflns_theta_full        60.32
_diffrn_reflns_theta_max         60.32
_diffrn_reflns_theta_min         3.34
_exptl_absorpt_coefficient_mu    1.571
_exptl_absorpt_correction_T_max  0.9256
_exptl_absorpt_correction_T_min  0.9256
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.147
_exptl_crystal_description       block
_exptl_crystal_F_000             2650
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.279
_refine_diff_density_min         -0.162
_refine_diff_density_rms         0.037
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.006(12)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    'riding model'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     831
_refine_ls_number_reflns         9398
_refine_ls_number_restraints     83
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.0421
_refine_ls_R_factor_gt           0.0339
_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^)+(0.0368P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0728
_refine_ls_wR_factor_ref         0.0761
_reflns_number_gt                8416
_reflns_number_total             9398
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja049462tsi20040727_101411.cif
_cod_data_source_block           compound2
_cod_original_formula_sum        'C72.65 H108.90 Al2 N4 O0.45 S2 Si2'
_cod_database_code               4112885