A trinuclear Zn3(OAc)4-3,3'-bis(aminoimino)binaphthoxide complex for highly efficient catalytic asymmetric iodolactonization
Takayoshi Arai; Noriyuki Sugiyama; Hyuma Masu; Sayaka Kado; Shinnosuke Yabe; Masahiro Yamanaka; Chem.Commun. 50 (2014) 8287–; doi:10.1039/C4cc02415J

data_7115320
_publ_section_title
;
 A trinuclear Zn3(OAc)4-3,3'-bis(aminoimino)binaphthoxide complex for
 highly efficient catalytic asymmetric iodolactonization
;
_journal_name_full               Chem.Commun.
_journal_page_first              8287
_journal_paper_doi               10.1039/C4cc02415J
_journal_volume                  50
_journal_year                    2014
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C74 H64 N4 O10 Zn3, 2(C H4 O), 6(O)'
_chemical_formula_sum            'C76 H72 N4 O18 Zn3'
_chemical_formula_weight         1525.49
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 108.310(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   11.1670(16)
_cell_length_b                   22.145(3)
_cell_length_c                   16.594(2)
_cell_measurement_reflns_used    2945
_cell_measurement_temperature    173
_cell_measurement_theta_max      25.03
_cell_measurement_theta_min      2.25
_cell_volume                     3895.8(9)
_computing_cell_refinement       'APEX2 (Bruker AXS, 2006)'
_computing_data_collection       'APEX2 (Bruker AXS, 2006)'
_computing_data_reduction        'SAINT (Bruker AXS, 2004)'
_computing_molecular_graphics    'XSHEL (Bruker AXS,2002)'
_computing_publication_material  'XCIF (Bruker AXS, 2001)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      173
_diffrn_detector_area_resol_mean 8.333
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.964
_diffrn_measurement_device_type  'Bruker APEXII 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  0.1230
_diffrn_reflns_av_sigmaI/netI    0.0638
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            20839
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         27.47
_diffrn_reflns_theta_min         1.92
_exptl_absorpt_coefficient_mu    0.984
_exptl_absorpt_correction_T_max  0.9525
_exptl_absorpt_correction_T_min  0.7568
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
SADABS Sheldrick 1996
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.300
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             1580
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.576
_refine_diff_density_min         -0.615
_refine_diff_density_rms         0.086
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.019(12)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     929
_refine_ls_number_reflns         15718
_refine_ls_number_restraints     121
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.0552
_refine_ls_R_factor_gt           0.0464
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0598P)^2^+0.7258P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1093
_refine_ls_wR_factor_ref         0.1139
_reflns_number_gt                11920
_reflns_number_total             15718
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4cc02415j2.cif
_cod_data_source_block           arai41_twin5
_cod_original_cell_volume        3896.0(9)
_cod_original_sg_symbol_H-M      'P2(1)   '
_cod_database_code               7115320