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_4035403
_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         '2(C2 H8 N1), Zn Cl4'
_chemical_formula_sum            'C4 H16 Cl4 N2 Zn'
_chemical_formula_weight         299.36
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.000(3)
_cell_angle_beta                 89.932(3)
_cell_angle_gamma                90.000(2)
_cell_formula_units_Z            4
_cell_length_a                   8.5348(5)
_cell_length_b                   11.4450(6)
_cell_length_c                   13.2997(8)
_cell_measurement_reflns_used    1349
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      0.9
_cell_volume                     1299.12(13)
_computing_structure_refinement  'SHELXL (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.99
_diffrn_measured_fraction_theta_max 0.99
_diffrn_measurement_device       '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  0.1377
_diffrn_reflns_av_sigmaI/netI    0.1137
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            7948
_diffrn_reflns_theta_full        27.5
_diffrn_reflns_theta_max         27.5
_diffrn_reflns_theta_min         2.3
_exptl_absorpt_coefficient_mu    2.669
_exptl_absorpt_correction_T_max  0.89
_exptl_absorpt_correction_T_min  0.71
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details
;
By Gaussian integration based on twelve indexed crystal faces (NUMABS;
Coppens, 1970)
;
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    1.531
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Plate
_exptl_crystal_F_000             608
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.876
_refine_diff_density_min         -0.713
_refine_diff_density_rms         0.149
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     100
_refine_ls_number_reflns         2980
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.1022
_refine_ls_R_factor_gt           0.0654
_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^)+(0.0777P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1478
_refine_ls_wR_factor_ref         0.1683
_reflns_d_resolution_high        0.7675
_reflns_number_gt                1976
_reflns_number_total             2980
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            jo8b01687_si_002.cif
_cod_data_source_block           sb_54
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4035403
_shelx_title                     ' Compound SB_54'
_shelx_refln_list_code           4
_shelx_f_calc_maximum            205.55
_shelx_f_squared_multiplier      1.000