Pair of chiral 2D silver(i) enantiomers: chiral recognition of l- and d-histidine via differential pulse voltammetry
Kim, Dongwon; Seo, Kyeong-Deok; Shim, Yoon-Bo; Lee, Kyungsuh; Lee, Sang Hak; Lee, Young-A.; Jung, Ok-Sang; Dalton Transactions  (2022) –; doi:10.1039/D1DT03371A

data_7709865
_publ_section_title
;
 Pair of chiral 2D silver(i) enantiomers: chiral recognition of l- and
 d-histidine via differential pulse voltammetry
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D1DT03371A
_journal_year                    2022
_chemical_formula_moiety         'C54 H42 Ag N6 O9, F6 P, 3(C4 H8 O2), O0.50'
_chemical_formula_sum            'C66 H67 Ag F6 N6 O15.5 P'
_chemical_formula_weight         1445.09
_space_group_crystal_system      triclinic
_space_group_IT_number           1
_space_group_name_Hall           'P 1'
_space_group_name_H-M_alt        'P 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_method           SHELXL-2019/2
_audit_update_record
;
2022-03-24 deposited with the CCDC.	2022-03-28 downloaded from the CCDC.
;
_cell_angle_alpha                67.17(3)
_cell_angle_beta                 72.20(3)
_cell_angle_gamma                87.20(3)
_cell_formula_units_Z            1
_cell_length_a                   10.284(2)
_cell_length_b                   12.348(3)
_cell_length_c                   14.787(3)
_cell_measurement_reflns_used    16948
_cell_measurement_temperature    223(2)
_cell_measurement_theta_max      33.858
_cell_measurement_theta_min      0.447
_cell_volume                     1642.6(8)
_computing_cell_refinement       'HKL3000sm (Otwinowski & Minor, 1997)'
_computing_data_collection       'PAL BL2D-SMDC Program (Shin et. al, 2016)'
_computing_data_reduction        'HKL3000sm (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'Mercury 4.2.0'
_computing_publication_material  'SHELXL-2019/2 (Sheldrick, 2019)'
_computing_structure_refinement  'SHELXL-2019/2 (Sheldrick, 2019)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      223(2)
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device_type  'Rayonix MX225HS CCD area detector'
_diffrn_measurement_method       'omega scan'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.780
_diffrn_reflns_av_R_equivalents  0.1127
_diffrn_reflns_av_unetI/netI     0.0959
_diffrn_reflns_Laue_measured_fraction_full 0.986
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_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            50248
_diffrn_reflns_point_group_measured_fraction_full 0.956
_diffrn_reflns_point_group_measured_fraction_max 0.956
_diffrn_reflns_theta_full        27.699
_diffrn_reflns_theta_max         27.699
_diffrn_reflns_theta_min         1.726
_diffrn_source                   'PLSII 2D bending magnet'
_exptl_absorpt_coefficient_mu    0.529
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.820
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'HKL3000sm Scalepack(Otwinowski et.al,2003)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.461
_exptl_crystal_description       block
_exptl_crystal_F_000             745
_exptl_crystal_size_max          0.023
_exptl_crystal_size_mid          0.021
_exptl_crystal_size_min          0.011
_refine_diff_density_max         0.737
_refine_diff_density_min         -0.409
_refine_diff_density_rms         0.066
_refine_ls_abs_structure_details
;
 Flack x determined using 1603 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.02(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.966
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     865
_refine_ls_number_reflns         11139
_refine_ls_number_restraints     146
_refine_ls_restrained_S_all      0.965
_refine_ls_R_factor_all          0.1911
_refine_ls_R_factor_gt           0.0870
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1551P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2246
_refine_ls_wR_factor_ref         0.2885
_reflns_Friedel_coverage         0.939
_reflns_Friedel_fraction_full    0.926
_reflns_Friedel_fraction_max     0.926
_reflns_number_gt                4458
_reflns_number_total             11139
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt03371a2.cif
_cod_data_source_block           AgPF6_BTII2
_cod_original_cell_volume        1642.6(7)
_cod_original_formula_sum        'C66 H67 Ag F6 N6 O15.50 P'
_cod_database_code               7709865
_shelx_shelxl_version_number     2019/2
_shelx_estimated_absorpt_t_min   0.988
_shelx_estimated_absorpt_t_max   0.994
_shelx_res_checksum              33182
_shelx_hkl_checksum              25828