Interrogation of fractional crystallization behavior of a newly exploited chiral resolution method for racemic 1-(pyridin-2-yl)ethylamine via DFT-D3 calculations of cohesive energy
Cho, Juhyun; Jeong, Jong Hwa; Lee, Myung Won; Kang, Youn K.; Inorganic Chemistry Frontiers 6 (2019) 2325–; doi:10.1039/C9QI00523D

data_4350047
_publ_section_title
;
 Interrogation of fractional crystallization behavior of a newly exploited
 chiral resolution method for racemic 1-(pyridin-2-yl)ethylamine via
 DFT-D3 calculations of cohesive energy
;
_journal_issue                   9
_journal_name_full               'Inorganic Chemistry Frontiers'
_journal_page_first              2325
_journal_paper_doi               10.1039/C9QI00523D
_journal_volume                  6
_journal_year                    2019
_chemical_absolute_configuration rmad
_chemical_formula_moiety         'C34 H48 Cl4 N4 Zn2, H2 C2 Cl6'
_chemical_formula_sum            'C36 H50 Cl10 N4 Zn2'
_chemical_formula_weight         1024.08
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2018/1
_audit_update_record
;
2019-05-08 deposited with the CCDC.	2019-07-11 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 93.677(8)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   12.7939(15)
_cell_length_b                   13.5872(10)
_cell_length_c                   13.4322(9)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      13.54
_cell_measurement_theta_min      11.32
_cell_volume                     2330.2(4)
_computing_cell_refinement       'CAD4 software (Enraf-Nonius. 1989)'
_computing_data_collection       'CAD4 software (Enraf-Nonius. 1989)'
_computing_data_reduction        'XCAD (McArdle, 1999)'
_computing_molecular_graphics    'ORTEXIII (McArdle, 1995)'
_computing_publication_material  'SHELXL-2018/1 (Sheldrick, 2018)'
_computing_structure_refinement  'SHELXL-2018/1 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Enraf-Nonius CAD4 4-circle diffractometer'
_diffrn_measurement_method       \w/2\q
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0550
_diffrn_reflns_av_unetI/netI     0.0417
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            9552
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.241
_diffrn_reflns_theta_max         25.484
_diffrn_reflns_theta_min         1.519
_diffrn_source                   'fine-focus sealed tube'
_diffrn_standards_interval_time  120
_diffrn_standards_number         1
_exptl_absorpt_coefficient_mu    1.633
_exptl_absorpt_correction_T_max  0.460
_exptl_absorpt_correction_T_min  0.457
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details   '(ABSCALC; McArdle & Daly, 1999)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.460
_exptl_crystal_description       brick
_exptl_crystal_F_000             1048
_exptl_crystal_size_max          0.500
_exptl_crystal_size_mid          0.480
_exptl_crystal_size_min          0.480
_exptl_transmission_factor_max   0.002
_exptl_transmission_factor_min   0.001
_refine_diff_density_max         0.971
_refine_diff_density_min         -0.608
_refine_diff_density_rms         0.074
_refine_ls_abs_structure_details
;
 Flack x determined using 2917 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.04(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.139
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     474
_refine_ls_number_reflns         8664
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.139
_refine_ls_R_factor_all          0.0713
_refine_ls_R_factor_gt           0.0497
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1414P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1640
_refine_ls_wR_factor_ref         0.1951
_reflns_Friedel_coverage         0.911
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.998
_reflns_number_gt                6739
_reflns_number_total             8675
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9qi00523d2.cif
_cod_data_source_block           '[RRSLZnCl2][RRRLZnCl2]'
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               4350047
_shelx_shelxl_version_number     2018/1
_shelx_estimated_absorpt_t_min   0.496
_shelx_estimated_absorpt_t_max   0.508
_shelx_res_checksum              33462
_shelx_hkl_checksum              95000