Mass spectrometric detection of enantioselectivity in three-component complexation, copper(ii)-chiral tetradentate ligand-free amino acid in solution.
Nakakoji, Takashi; Sato, Hirofumi; Ono, Daisuke; Miyake, Hiroyuki; Shinoda, Satoshi; Tsukube, Hiroshi; Kawasaki, Hideya; Arakawa, Ryuichi; Shizuma, Motohiro; Chemical communications (Cambridge, England) 56 (2019) 54–57; doi:10.1039/c9cc07231d

data_7124466
_publ_section_title
;
 Mass spectrometric detection of enantioselectivity in three-component
 complexation, copper(ii)-chiral tetradentate ligand-free amino acid in
 solution.
;
_journal_issue                   1
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              54
_journal_page_last               57
_journal_paper_doi               10.1039/c9cc07231d
_journal_volume                  56
_journal_year                    2019
_chemical_absolute_configuration rmad
_chemical_formula_moiety         'C14 H34 Cu N4 O4, 2(Cl O4), 2(C H4 O)'
_chemical_formula_sum            'C16 H42 Cl2 Cu N4 O14'
_chemical_formula_weight         648.97
_space_group_crystal_system      trigonal
_space_group_IT_number           154
_space_group_name_Hall           'P 32 2"'
_space_group_name_H-M_alt        'P 32 2 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2019-04-26 deposited with the CCDC.	2019-11-03 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            3
_cell_length_a                   8.729(9)
_cell_length_b                   8.729(9)
_cell_length_c                   33.58(4)
_cell_measurement_reflns_used    137
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.4835
_cell_measurement_theta_min      3.0312
_cell_volume                     2216(4)
_computing_cell_refinement       'CrystalClear (Rigaku Corp., 2000)'
_computing_data_collection       'CrystalClear (Rigaku Corp., 2000)'
_computing_data_reduction        'CrystalClear (Rigaku Corp., 2000)'
_computing_molecular_graphics    'Yadokari-XG (Wakita, Nemoto et al., 2009)'
_computing_publication_material  'Yadokari-XG (Wakita, Nemoto et al., 2009)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SIR2004 (Burla et al., 2004)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.972
_diffrn_measured_fraction_theta_max 0.975
_diffrn_measurement_device
;
Mercury CCD (2x2 bin mode)
;
_diffrn_measurement_method       \w
_diffrn_radiation_detector       CCD
_diffrn_radiation_monochromator  'Graphite Monochromator'
_diffrn_radiation_source         'Rotating Anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0465
_diffrn_reflns_av_unetI/netI     0.0339
_diffrn_reflns_Laue_measured_fraction_full 0.972
_diffrn_reflns_Laue_measured_fraction_max 0.975
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       41
_diffrn_reflns_limit_l_min       -43
_diffrn_reflns_number            16969
_diffrn_reflns_point_group_measured_fraction_full 0.971
_diffrn_reflns_point_group_measured_fraction_max 0.963
_diffrn_reflns_theta_full        25.241
_diffrn_reflns_theta_max         27.467
_diffrn_reflns_theta_min         3.252
_exptl_absorpt_coefficient_mu    0.986
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.8078
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(Jacobson, 1998)'
_exptl_crystal_colour            Blue
_exptl_crystal_density_diffrn    1.459
_exptl_crystal_description       Prism
_exptl_crystal_F_000             1023
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.300
_exptl_crystal_size_min          0.200
_refine_diff_density_max         0.284
_refine_diff_density_min         -0.434
_refine_diff_density_rms         0.088
_refine_ls_abs_structure_details
;
 Flack x determined using 1122 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.001(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.277
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     203
_refine_ls_number_reflns         3269
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.277
_refine_ls_R_factor_all          0.0448
_refine_ls_R_factor_gt           0.0415
_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^)+(0.0381P)^2^+0.9592P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0939
_refine_ls_wR_factor_ref         0.0971
_reflns_Friedel_coverage         0.664
_reflns_Friedel_fraction_full    0.969
_reflns_Friedel_fraction_max     0.947
_reflns_number_gt                3161
_reflns_number_total             3269
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9cc07231d2.cif
_cod_data_source_block           '[Cu(C12H26N4O2)(MeOH)2](ClO4)2(MeOH)2'
_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/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/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 

 Adding full bibliography for 7124466.cif.
;
_cod_original_cell_volume        2216(5)
_cod_database_code               7124466
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.756
_shelx_estimated_absorpt_t_max   0.827
_shelx_res_checksum              73251