Reactions of N-Monosubstituted Amidines with AlMe3and AlMeCl2: Formation of Fused Triazaalane Heterocycles
Maheswari, K.; Reddy, N. Dastagiri; Organometallics 31 (2012) 197–; doi:10.1021/om2007375

data_4067822
_publ_section_title
;
 Reactions of N-Monosubstituted Amidines with AlMe3and AlMeCl2: Formation
 of Fused Triazaalane Heterocycles
;
_journal_issue                   1
_journal_name_full               Organometallics
_journal_page_first              197
_journal_paper_doi               10.1021/om2007375
_journal_volume                  31
_journal_year                    2012
_chemical_formula_moiety         'C60 H92 Al4 N8, 0.5(C7 H8)'
_chemical_formula_sum            'C63.5 H96 Al4 N8'
_chemical_formula_weight         1079.40
_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                90.704(2)
_cell_angle_beta                 105.772(2)
_cell_angle_gamma                103.897(2)
_cell_formula_units_Z            4
_cell_length_a                   18.5489(3)
_cell_length_b                   18.6181(3)
_cell_length_c                   21.6897(4)
_cell_measurement_reflns_used    31817
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      29.3081
_cell_measurement_theta_min      2.7469
_cell_volume                     6973.3(2)
_computing_cell_refinement
;
'Mon Jul 18 22:48:45 2011'
;
_computing_data_collection
;
'Mon Jul 18 22:48:45 2011'
;
_computing_data_reduction
;
'Mon Jul 18 22:48:45 2011'
;
_computing_molecular_graphics    'ORTEP III & Olex 2.1'
_computing_publication_material  WinGX
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 15.9821
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Xcalibur, Eos'
_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  0.0531
_diffrn_reflns_av_sigmaI/netI    0.0744
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            64251
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.75
_exptl_absorpt_coefficient_mu    0.107
_exptl_absorpt_correction_T_max  0.9738
_exptl_absorpt_correction_T_min  0.9436
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
'Mon Jul 18 22:48:45 2011'
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.028
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2340
_exptl_crystal_size_max          0.55
_exptl_crystal_size_mid          0.45
_exptl_crystal_size_min          0.25
_refine_diff_density_max         1.725
_refine_diff_density_min         -0.534
_refine_diff_density_rms         0.085
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1354
_refine_ls_number_reflns         24508
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.1110
_refine_ls_R_factor_gt           0.0743
_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^)+(0.1410P)^2^+6.8714P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2259
_refine_ls_wR_factor_ref         0.2540
_reflns_number_gt                16561
_reflns_number_total             24508
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            om2007375_si_001.cif
_cod_data_source_block           Compound_3
_cod_depositor_comments
;

2025-11-10
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C127 H192 Al8 N16'
_cod_original_formula_weight         2158.81
_cod_original_formula_moiety         '2(C60 H92 Al4 N8), C7 H8'
_cod_original_formula_units_Z            2
_cod_database_code               4067822