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_4089282
_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         'C61 H95 Al N2 O2 Y, C6 H18 O Si2'
_chemical_formula_sum            'C67 H113 Al N2 O3 Si2 Y'
_chemical_formula_weight         1166.66
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 101.616(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   21.812(3)
_cell_length_b                   12.0055(19)
_cell_length_c                   27.328(4)
_cell_measurement_reflns_used    6609
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      20.60
_cell_measurement_theta_min      2.16
_cell_volume                     7009.7(18)
_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 0.995
_diffrn_measured_fraction_theta_max 0.995
_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  0.1460
_diffrn_reflns_av_unetI/netI     0.1362
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            61948
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        24.760
_diffrn_reflns_theta_max         24.760
_diffrn_reflns_theta_min         1.521
_exptl_absorpt_coefficient_mu    0.920
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.7679
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.105
_exptl_crystal_description       rod
_exptl_crystal_F_000             2532
_exptl_crystal_size_max          0.272
_exptl_crystal_size_mid          0.142
_exptl_crystal_size_min          0.110
_refine_diff_density_max         0.833
_refine_diff_density_min         -1.396
_refine_diff_density_rms         0.102
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     675
_refine_ls_number_reflns         11965
_refine_ls_number_restraints     669
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.1998
_refine_ls_R_factor_gt           0.1233
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0574P)^2^+75.1104P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2467
_refine_ls_wR_factor_ref         0.2819
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6922
_reflns_number_total             11965
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om7b00156_si_002.cif
_cod_data_source_block           xn2ytmsal_0m_a
_cod_original_cell_volume        7009.9(19)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4089282
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.788
_shelx_estimated_absorpt_t_max   0.906
_shelx_res_checksum              5614
_shelx_hkl_checksum              18236