Preparative-Scale Synthesis of Vedejs Chiral DMAP Catalysts.
Kinens, Artis; Balkaitis, Simonas; Suna, Edgars; The Journal of organic chemistry 83 (2018) 12449–12459; doi:10.1021/acs.joc.8b01687

data_4035401
_publ_section_title
;
 Preparative-Scale Synthesis of Vedejs Chiral DMAP Catalysts.
;
_journal_issue                   20
_journal_name_full               'The Journal of organic chemistry'
_journal_page_first              12449
_journal_page_last               12459
_journal_paper_doi               10.1021/acs.joc.8b01687
_journal_volume                  83
_journal_year                    2018
_chemical_formula_moiety         'C8 H18 Cl2 N2 Zn'
_chemical_formula_sum            'C8 H18 Cl2 N2 Zn'
_chemical_formula_weight         278.51
_space_group_IT_number           60
_space_group_name_Hall           '-P 2b 2ac'
_space_group_name_H-M_alt        'P c n b'
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   'P c n b'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   6.9330(2)
_cell_length_b                   17.2571(4)
_cell_length_c                   20.0543(5)
_cell_measurement_reflns_used    2096
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      0.9
_cell_volume                     2399.37(11)
_computing_structure_refinement  'SHELXL (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.98
_diffrn_measured_fraction_theta_max 0.98
_diffrn_measurement_device_type  'Bruker-Nonius KappaCCD'
_diffrn_measurement_method       '\f and \w scan'
_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  0.0433
_diffrn_reflns_av_sigmaI/netI    0.0498
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            5760
_diffrn_reflns_theta_full        29.0
_diffrn_reflns_theta_max         29.0
_diffrn_reflns_theta_min         2.0
_exptl_absorpt_coefficient_mu    2.453
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    1.542
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prism
_exptl_crystal_F_000             1152
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.949
_refine_diff_density_min         -2.979
_refine_diff_density_rms         0.225
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.225
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     155
_refine_ls_number_reflns         3097
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.225
_refine_ls_R_factor_all          0.1316
_refine_ls_R_factor_gt           0.1087
_refine_ls_shift/su_max          0.097
_refine_ls_shift/su_mean         0.011
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+72.4698P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2603
_refine_ls_wR_factor_ref         0.2686
_reflns_d_resolution_high        0.7402
_reflns_number_gt                2387
_reflns_number_total             3097
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            jo8b01687_si_003.cif
_cod_data_source_block           AK383a
_cod_database_code               4035401
_shelx_title                     ' Compound ak-341'
_shelx_refln_list_code           4
_shelx_f_calc_maximum            327.57
_shelx_f_squared_multiplier      1.000