Dearomatization and Functionalization of Terpyridine Ligands Leading to Unprecedented Zwitterionic Meisenheimer Aluminum Complexes and Their Use in Catalytic Hydroboration
Zhang, Guoqi; Wu, Jing; Zeng, Haisu; Neary, Michelle C.; Devany, Matthew; Zheng, Shengping; Dub, Pavel A.; ACS Catalysis 9 (2018) 874–; doi:10.1021/acscatal.8b04096

data_4515492
_publ_section_title
;
 Dearomatization and Functionalization of Terpyridine Ligands Leading to
 Unprecedented Zwitterionic Meisenheimer Aluminum Complexes and Their Use
 in Catalytic Hydroboration
;
_journal_issue                   2
_journal_name_full               'ACS Catalysis'
_journal_page_first              874
_journal_paper_doi               10.1021/acscatal.8b04096
_journal_volume                  9
_journal_year                    2018
_chemical_formula_moiety         'C32 H41 Al N4, 0.5(C6 H6)'
_chemical_formula_sum            'C35 H44 Al N4'
_chemical_formula_weight         547.72
_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
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                91.033(2)
_cell_angle_beta                 97.953(2)
_cell_angle_gamma                107.345(2)
_cell_formula_units_Z            2
_cell_length_a                   9.0364(3)
_cell_length_b                   10.9957(4)
_cell_length_c                   16.5417(6)
_cell_measurement_reflns_used    9898
_cell_measurement_temperature    130(2)
_cell_measurement_theta_max      30.08
_cell_measurement_theta_min      2.37
_cell_volume                     1550.72(10)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      130(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0894
_diffrn_reflns_av_unetI/netI     0.0959
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            54378
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         30.477
_diffrn_reflns_theta_min         2.582
_exptl_absorpt_coefficient_mu    0.095
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.7035
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.173
_exptl_crystal_description       plate
_exptl_crystal_F_000             590
_exptl_crystal_size_max          0.230
_exptl_crystal_size_mid          0.220
_exptl_crystal_size_min          0.050
_refine_diff_density_max         0.383
_refine_diff_density_min         -0.323
_refine_diff_density_rms         0.060
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.011
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     367
_refine_ls_number_reflns         9388
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.011
_refine_ls_R_factor_all          0.1333
_refine_ls_R_factor_gt           0.0585
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0446P)^2^+0.6903P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1091
_refine_ls_wR_factor_ref         0.1342
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5359
_reflns_number_total             9388
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cs8b04096_si_010.cif
_cod_data_source_block           gz1185
_cod_database_code               4515492
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.978
_shelx_estimated_absorpt_t_max   0.995
_shelx_res_checksum              64459
_shelx_hkl_checksum              67466