Yttrium and Aluminum Alkyl Complexes of a Rigid Bis-Anilido NON-Donor Ligand: Synthesis and Hydroamination Catalysis
Motolko, Kelly S. A.; Emslie, David J. H.; Jenkins, Hilary A.; Organometallics 36 (2017) 1601–; doi:10.1021/acs.organomet.7b00156

data_4089283
_publ_section_title
;
 Yttrium and Aluminum Alkyl Complexes of a Rigid Bis-Anilido NON-Donor
 Ligand: Synthesis and Hydroamination Catalysis
;
_journal_issue                   8
_journal_name_full               Organometallics
_journal_page_first              1601
_journal_paper_doi               10.1021/acs.organomet.7b00156
_journal_volume                  36
_journal_year                    2017
_chemical_formula_moiety         '2(C54 H77 Al N2 O), C6 H18 O Si2'
_chemical_formula_sum            'C114 H172 Al2 N4 O3 Si2'
_chemical_formula_weight         1756.69
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-I 2ya'
_space_group_name_H-M_alt        'I 1 2/a 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 108.901(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.330(2)
_cell_length_b                   29.736(2)
_cell_length_c                   20.4953(14)
_cell_measurement_reflns_used    6438
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      24.39
_cell_measurement_theta_min      2.23
_cell_volume                     11145.4(16)
_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      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.998
_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  0.0414
_diffrn_reflns_av_unetI/netI     0.0567
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       36
_diffrn_reflns_limit_k_min       -37
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            47064
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         26.407
_diffrn_reflns_theta_min         1.860
_exptl_absorpt_coefficient_mu    0.096
_exptl_absorpt_correction_T_max  24.389
_exptl_absorpt_correction_T_min  2.226
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.047
_exptl_crystal_description       kite
_exptl_crystal_F_000             3848
_exptl_crystal_size_max          0.583
_exptl_crystal_size_mid          0.345
_exptl_crystal_size_min          0.074
_refine_diff_density_max         0.318
_refine_diff_density_min         -0.397
_refine_diff_density_rms         0.045
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     591
_refine_ls_number_reflns         11425
_refine_ls_number_restraints     21
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.0842
_refine_ls_R_factor_gt           0.0522
_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^)+(0.0489P)^2^+12.5805P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1249
_refine_ls_wR_factor_ref         0.1427
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7908
_reflns_number_total             11425
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om7b00156_si_002.cif
_cod_data_source_block           k_a
_cod_original_cell_volume        11145.7(16)
_cod_original_sg_symbol_H-M      'I 2/a'
_cod_database_code               4089283
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.946
_shelx_estimated_absorpt_t_max   0.993
_shelx_res_checksum              5152
_shelx_hkl_checksum               31525