Redox Routes to Substitution of Aluminum(III): Synthesis and Characterization of (IP-)2AlX (IP = α-iminopyridine, X = Cl, Me, SMe, S2CNMe2, C\τbCPh, N3, SPh, NHPh)
Thomas W. Myers; Alexandra L. Holmes; Louise A. Berben; Inorganic Chemistry 51 (2012) 8997–9004; doi:10.1021/ic301128m

data_4330071
_publ_section_title
;
 Redox Routes to Substitution of Aluminum(III): Synthesis and
 Characterization of (IP-)2AlX (IP = \a-iminopyridine, X = Cl, Me, SMe,
 S2CNMe2, C\\tbCPh, N3, SPh, NHPh)
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              8997
_journal_page_last               9004
_journal_paper_doi               10.1021/ic301128m
_journal_volume                  51
_journal_year                    2012
_chemical_formula_sum            'C64 H99.2 Al N4 Na O7'
_chemical_formula_weight         1086.64
_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-97
_cell_angle_alpha                90.00
_cell_angle_beta                 102.6160(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.7939(8)
_cell_length_b                   15.6454(7)
_cell_length_c                   22.9473(11)
_cell_measurement_reflns_used    100
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      28.54
_cell_measurement_theta_min      2.94
_cell_volume                     6234.1(5)
_computing_cell_refinement       'Bruker APEX'
_computing_data_collection       'Bruker APEX'
_computing_data_reduction        'Bruker Saint'
_computing_molecular_graphics    'Bruker Shelxtl'
_computing_publication_material  'Bruker Shelxtl'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      90(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega 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  0.0429
_diffrn_reflns_av_sigmaI/netI    0.0327
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            56726
_diffrn_reflns_theta_full        25.13
_diffrn_reflns_theta_max         25.13
_diffrn_reflns_theta_min         2.33
_exptl_absorpt_coefficient_mu    0.093
_exptl_absorpt_correction_T_max  0.9968
_exptl_absorpt_correction_T_min  0.9669
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            Purple
_exptl_crystal_density_diffrn    1.158
_exptl_crystal_description       Block
_exptl_crystal_F_000             2365
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.22
_refine_diff_density_max         0.587
_refine_diff_density_min         -0.556
_refine_diff_density_rms         0.049
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.981
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     712
_refine_ls_number_reflns         11124
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.981
_refine_ls_R_factor_all          0.0717
_refine_ls_R_factor_gt           0.0492
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0655P)^2^+5.6711P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1239
_refine_ls_wR_factor_ref         0.1388
_reflns_number_gt                8342
_reflns_number_total             11124
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic301128m_si_002_1.cif
_cod_data_source_block           twm62
_cod_original_formula_sum        'C64 H99.20 Al N4 Na O7'
_cod_database_code               4330071