Discrimination of Enantiomers of Dipeptide Derivatives with Two Chiral Centers by Tetraaza Macrocyclic Chiral Solvating Agents Using <sup>1</sup>H NMR Spectroscopy.
Fang, Lixia; Lv, Caixia; Wang, Guo; Feng, Lei; Stavropoulos, Pericles; Gao, Guangpeng; Ai, Lin; Zhang, Jiaxin; Organic chemistry frontiers : an international journal of organic chemistry 3 (2016) 1716–1724; doi:10.1039/C6QO00521G

data_4036723
_publ_section_title
;
 Discrimination of Enantiomers of Dipeptide Derivatives with Two Chiral
 Centers by Tetraaza Macrocyclic Chiral Solvating Agents Using
 <sup>1</sup>H NMR Spectroscopy.
;
_journal_issue                   12
_journal_name_full
'Organic chemistry frontiers : an international journal of organic chemistry'
_journal_page_first              1716
_journal_page_last               1724
_journal_paper_doi               10.1039/C6QO00521G
_journal_volume                  3
_journal_year                    2016
_chemical_absolute_configuration rmad
_chemical_formula_sum            'C37 H36 Br2 Cl3 D N4 O4'
_chemical_formula_weight         868.88
_space_group_crystal_system      tetragonal
_space_group_IT_number           78
_space_group_name_Hall           'P 4cw'
_space_group_name_H-M_alt        'P 43'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2013
_audit_update_record
;
2014-06-06 deposited with the CCDC.
2016-10-05 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.811(3)
_cell_length_b                   13.811(3)
_cell_length_c                   20.076(4)
_cell_measurement_reflns_used    9179
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.17
_cell_measurement_theta_min      2.51
_cell_volume                     3829.4(14)
_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-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0384
_diffrn_reflns_av_unetI/netI     0.0575
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            25246
_diffrn_reflns_point_group_measured_fraction_full 0.914
_diffrn_reflns_point_group_measured_fraction_max 0.897
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.514
_diffrn_reflns_theta_min         1.790
_exptl_absorpt_coefficient_mu    2.370
_exptl_absorpt_correction_T_max  0.75
_exptl_absorpt_correction_T_min  0.59
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_density_diffrn    1.507
_exptl_crystal_F_000             1760
_exptl_crystal_size_max          0.500
_exptl_crystal_size_mid          0.180
_exptl_crystal_size_min          0.110
_refine_diff_density_max         0.704
_refine_diff_density_min         -0.663
_refine_diff_density_rms         0.058
_refine_ls_abs_structure_details
; 
 Flack x determined using 2710 quotients [(I+)-(I-)]/[(I+)+(I-)] 
 (Parsons and Flack (2004), Acta Cryst. A60, s61). 
;
_refine_ls_abs_structure_Flack   0.023(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     465
_refine_ls_number_reflns         7907
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.0397
_refine_ls_R_factor_gt           0.0317
_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^)+(0.0238P)^2^+0.5870P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0679
_refine_ls_wR_factor_ref         0.0706
_reflns_Friedel_coverage         0.748
_reflns_Friedel_fraction_full    0.823
_reflns_Friedel_fraction_max     0.790
_reflns_number_gt                7020
_reflns_number_total             7907
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6qo00521g2.cif
_cod_data_source_block           131202a_0m
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_exptl_absorpt_correction_type' value 'Multi-scan' was
changed to 'multi-scan' in accordance with the
/home/saulius/struct/COD-crude-data/automatic-downloads/DataCite-retrospective/RSC/depositions/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 6909 2019-04-08 15:41:33Z antanas 
;
_cod_original_cell_volume        3829.5(16)
_cod_original_formula_sum        'C37 H36 D Br2 Cl3 N4 O4'
_cod_database_code               4036723
_shelx_estimated_absorpt_t_min   0.384
_shelx_estimated_absorpt_t_max   0.781