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_7116810
_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_formula_sum            'C72 H87 N5 O4 Zr2'
_chemical_formula_weight         1268.91
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_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                100.831(3)
_cell_angle_beta                 93.008(3)
_cell_angle_gamma                111.473(3)
_cell_formula_units_Z            2
_cell_length_a                   12.0652(19)
_cell_length_b                   13.096(2)
_cell_length_c                   23.377(4)
_cell_measurement_reflns_used    6988
_cell_measurement_temperature    133(2)
_cell_measurement_theta_max      25.08
_cell_measurement_theta_min      2.38
_cell_volume                     3346.2(9)
_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-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      133(2)
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w 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  0.0461
_diffrn_reflns_av_sigmaI/netI    0.0814
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            21203
_diffrn_reflns_theta_full        25.10
_diffrn_reflns_theta_max         25.10
_diffrn_reflns_theta_min         1.75
_exptl_absorpt_coefficient_mu    0.362
_exptl_absorpt_correction_T_max  0.9892
_exptl_absorpt_correction_T_min  0.9579
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.259
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1332
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.03
_platon_squeeze_details
;
;
_refine_diff_density_max         1.191
_refine_diff_density_min         -0.782
_refine_diff_density_rms         0.106
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.953
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     748
_refine_ls_number_reflns         11728
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      0.954
_refine_ls_R_factor_all          0.0791
_refine_ls_R_factor_gt           0.0483
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0814P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1250
_refine_ls_wR_factor_ref         0.1389
_reflns_number_gt                8134
_reflns_number_total             11728
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4cc10032h2.cif
_cod_data_source_block           9
_cod_original_cell_volume        3346.3(9)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7116810