Molecular Structures and Redox Properties of Homoleptic Aluminum(III) Complexes with Azobisphenolate (azp) Ligands
Takahashi, Kazuyuki; Noguchi, Takumi; Ueda, Keiji; Miyawaki, Atsuhiro; Murata, Suguru; Inorganics 10 (2022) 84–; doi:10.3390/inorganics10060084

data_1567243
_publ_section_title
;
 Molecular Structures and Redox Properties of Homoleptic Aluminum(III)
 Complexes with Azobisphenolate (azp) Ligands
;
_journal_issue                   6
_journal_name_full               Inorganics
_journal_page_first              84
_journal_paper_doi               10.3390/inorganics10060084
_journal_volume                  10
_journal_year                    2022
_chemical_formula_sum            'C53 H48 Al N4 O6 P'
_chemical_formula_weight         894.93
_chemical_name_common            (TPP)[Al(azpMe2)2]
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_cell_angle_alpha                81.934(2)
_cell_angle_beta                 81.586(2)
_cell_angle_gamma                64.230(2)
_cell_formula_units_Z            2
_cell_length_a                   11.8738(19)
_cell_length_b                   13.224(2)
_cell_length_c                   16.406(3)
_cell_measurement_reflns_used    6162
_cell_measurement_temperature    90.(2)
_cell_measurement_theta_max      28.2293
_cell_measurement_theta_min      2.1878
_cell_volume                     2286.4(7)
_computing_molecular_graphics    'shelXle (C.B. Huebschle, rev 958)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      90.(2)
_diffrn_measured_fraction_theta_full 0.968
_diffrn_measured_fraction_theta_max 0.968
_diffrn_measurement_device_type  'Bruker APEXII CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  'Bruker Helios multilayer confocal mirror'
_diffrn_radiation_source         'Bruker TXS fine-focus rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0173
_diffrn_reflns_av_unetI/netI     0.0353
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            12543
_diffrn_reflns_theta_full        26.73
_diffrn_reflns_theta_max         26.73
_diffrn_reflns_theta_min         1.96
_diffrn_source                   'rotating-anode X-ray tube'
_diffrn_source_type              'Bruker Turbo X-ray Source'
_exptl_absorpt_coefficient_mu    0.136
_exptl_absorpt_correction_T_max  0.99
_exptl_absorpt_correction_T_min  0.97
_exptl_absorpt_process_details
;
;
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_diffrn    1.300
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             940
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.170
_exptl_crystal_size_min          0.120
_refine_diff_density_max         1.873
_refine_diff_density_min         -0.820
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     739
_refine_ls_number_reflns         9378
_refine_ls_number_restraints     887
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.0843
_refine_ls_R_factor_gt           0.0703
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1020P)^2^+3.4825P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1902
_refine_ls_wR_factor_ref         0.2036
_reflns_number_gt                7563
_reflns_number_total             9378
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            1-Me2.cif
_cod_data_source_block           TPP_Al_azpMe2_90K
_cod_original_cell_volume        2286.4(6)
_cod_database_code               1567243
_shelx_res_checksum              19719
_shelx_hkl_checksum              36412