Asymmetric hydroamination catalyzed by a new chiral zirconium system: reaction scope and mechanism
Xiaoguang Zhou; Bing Wei; Xiu-Li Sun; Yong Tang; Zuowei Xie; Chem.Commun. 51 (2015) 5751–; doi:10.1039/C4cc10032H

data_7116799
_publ_section_title
;
 Asymmetric hydroamination catalyzed by a new chiral zirconium system:
 reaction scope and mechanism
;
_journal_name_full               Chem.Commun.
_journal_page_first              5751
_journal_paper_doi               10.1039/C4cc10032H
_journal_volume                  51
_journal_year                    2015
_chemical_absolute_configuration ad
_chemical_formula_sum            'C42 H57 N O2 Zr'
_chemical_formula_weight         699.11
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           145
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  'P 32'
_symmetry_space_group_name_H-M   'P 32'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2014-07-26 deposited with the CCDC.
2015-02-19 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            9
_cell_length_a                   25.473(4)
_cell_length_b                   25.473(4)
_cell_length_c                   15.017(3)
_cell_measurement_reflns_used    9202
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      54.339
_cell_measurement_theta_min      4.885
_cell_volume                     8439(3)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0197
_diffrn_reflns_av_sigmaI/netI    0.0238
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            62219
_diffrn_reflns_theta_full        26.49
_diffrn_reflns_theta_max         26.49
_diffrn_reflns_theta_min         1.60
_exptl_absorpt_coefficient_mu    0.328
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_correction_T_min  0.6325
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.238
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             3348
_exptl_crystal_size_max          0.369
_exptl_crystal_size_mid          0.311
_exptl_crystal_size_min          0.257
_refine_diff_density_max         1.623
_refine_diff_density_min         -1.024
_refine_diff_density_rms         0.140
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.12(5)
_refine_ls_extinction_coef       0.00076(12)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.128
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1244
_refine_ls_number_reflns         22434
_refine_ls_number_restraints     20
_refine_ls_restrained_S_all      1.129
_refine_ls_R_factor_all          0.0897
_refine_ls_R_factor_gt           0.0888
_refine_ls_shift/su_max          0.013
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0521P)^2^+73.0683P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2347
_refine_ls_wR_factor_ref         0.2352
_reflns_number_gt                22064
_reflns_number_total             22434
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4cc10032h2.cif
_cod_data_source_block           2
_cod_original_cell_volume        8439(2)
_cod_original_sg_symbol_H-M      P3(2)
_cod_database_code               7116799