Selective and Nonselective Aza-Michael Additions Catalyzed by a Chiral Zirconium Bis-Diketiminate Complex
El-Zoghbi, Ibrahim; Kebdani, Myriam; Whitehorne, Todd J. J.; Schaper, Frank; Organometallics 32 (2013) 6986–; doi:10.1021/om400544z

data_4081793
_publ_section_title
;
 Selective and Nonselective Aza-Michael Additions Catalyzed by a Chiral
 Zirconium Bis-Diketiminate Complex
;
_journal_issue                   23
_journal_name_full               Organometallics
_journal_page_first              6986
_journal_paper_doi               10.1021/om400544z
_journal_volume                  32
_journal_year                    2013
_chemical_compound_source        'Synthesized by the authors. See text'
_chemical_formula_sum            'C34 H42 F6 N4 O6 S2 Zr'
_chemical_formula_weight         872.05
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           33
_space_group_name_Hall           'P 2c -2n'
_space_group_name_H-M_alt        'P n a 21'
_symmetry_space_group_name_Hall  'P 2c -2n'
_symmetry_space_group_name_H-M   'P n a 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   38.0942(10)
_cell_length_b                   11.4367(4)
_cell_length_c                   17.0337(5)
_cell_measurement_reflns_used    7542
_cell_measurement_temperature    100
_cell_measurement_theta_max      69.92
_cell_measurement_theta_min      3.48
_cell_volume                     7421.1(4)
_computing_cell_refinement       'SAINT V8.30C(Bruker AXS)'
_computing_data_collection       'APEX2  (Bruker AXS)'
_computing_data_reduction        'SAINT V8.30C(Bruker AXS)'
_computing_molecular_graphics    'SHELXTL  (Bruker AXS, 2003)'
_computing_publication_material  'UdMX (Maris, 2004)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100
_diffrn_detector_area_resol_mean 8.3
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker APEX II'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  'Quazar MX'
_diffrn_radiation_source         'Incoatec I\muS Microsource '
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.095
_diffrn_reflns_av_unetI/netI     0.0584
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       46
_diffrn_reflns_limit_h_min       -46
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            103102
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         71.867
_diffrn_reflns_theta_min         2.320
_exptl_absorpt_coefficient_mu    4.186
_exptl_absorpt_correction_T_max  0.7535
_exptl_absorpt_correction_T_min  0.5817
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Sadabs (Sheldrick, 2012)'
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.561
_exptl_crystal_description       block
_exptl_crystal_F_000             3584
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.06
_refine_ls_abs_structure_details
'Flack, H.D. and Schwarzenbach, D. (1999), XXXX Friedel Pairs'
_refine_ls_abs_structure_Flack   0.32(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     972
_refine_ls_number_reflns         14451
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.0847
_refine_ls_R_factor_gt           0.0728
_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^)+(0.1495P)^2^+1.0871P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1882
_refine_ls_wR_factor_ref         0.2023
_reflns_Friedel_coverage         0.931
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.996
_reflns_number_gt                12216
_reflns_number_total             14451
_cod_data_source_file            om400544z_si_002.cif
_cod_data_source_block           TODD31
_cod_original_sg_symbol_H-M      Pna21
_cod_database_code               4081793
_shelx_estimated_absorpt_t_min   0.731
_shelx_estimated_absorpt_t_max   0.787