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_4330072
_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            'C50 H78 Al N4 Na O6'
_chemical_formula_weight         881.13
_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                 126.148(11)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.780(4)
_cell_length_b                   16.551(4)
_cell_length_c                   22.569(4)
_cell_measurement_reflns_used    90
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      29.84
_cell_measurement_theta_min      2.54
_cell_volume                     5061(2)
_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 0.998
_diffrn_measured_fraction_theta_max 0.961
_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  0.0883
_diffrn_reflns_av_sigmaI/netI    0.1302
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            38559
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         30.49
_diffrn_reflns_theta_min         1.50
_exptl_absorpt_coefficient_mu    0.098
_exptl_absorpt_correction_T_max  0.9664
_exptl_absorpt_correction_T_min  0.8932
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            Purple
_exptl_crystal_density_diffrn    1.156
_exptl_crystal_description       Block
_exptl_crystal_F_000             1912
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.15
_refine_diff_density_max         2.392
_refine_diff_density_min         -0.734
_refine_diff_density_rms         0.130
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     575
_refine_ls_number_reflns         14814
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.022
_refine_ls_R_factor_all          0.2090
_refine_ls_R_factor_gt           0.1204
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1733P)^2^+10.2258P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3042
_refine_ls_wR_factor_ref         0.3598
_reflns_number_gt                7417
_reflns_number_total             14814
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic301128m_si_002_2.cif
_cod_data_source_block           jc3
_cod_original_cell_volume        5061.4(19)
_cod_database_code               4330072