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_7709864
_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), O'
_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                68.10(3)
_cell_angle_beta                 73.46(3)
_cell_angle_gamma                88.06(3)
_cell_formula_units_Z            1
_cell_length_a                   10.275(2)
_cell_length_b                   12.274(3)
_cell_length_c                   14.766(3)
_cell_measurement_reflns_used    58499
_cell_measurement_temperature    223(2)
_cell_measurement_theta_max      33.749
_cell_measurement_theta_min      0.401
_cell_volume                     1650.9(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 1.000
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  'Rayonix MX225HS CCD area detector'
_diffrn_measurement_method       'omega scan'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.700
_diffrn_reflns_av_R_equivalents  0.0792
_diffrn_reflns_av_unetI/netI     0.0696
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            54433
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.971
_diffrn_reflns_theta_full        24.835
_diffrn_reflns_theta_max         28.000
_diffrn_reflns_theta_min         1.531
_diffrn_source                   'PLSII 2D bending magnet'
_exptl_absorpt_coefficient_mu    0.396
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.498
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'HKL3000sm Scalepack(Otwinowski et.al,2003)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.454
_exptl_crystal_description       block
_exptl_crystal_F_000             745
_exptl_crystal_size_max          0.140
_exptl_crystal_size_mid          0.060
_exptl_crystal_size_min          0.055
_refine_diff_density_max         0.953
_refine_diff_density_min         -1.015
_refine_diff_density_rms         0.090
_refine_ls_abs_structure_details
;
 Flack x determined using 3934 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.015(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.920
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     865
_refine_ls_number_reflns         16199
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      0.920
_refine_ls_R_factor_all          0.0995
_refine_ls_R_factor_gt           0.0632
_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^)+(0.1206P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1625
_refine_ls_wR_factor_ref         0.1829
_reflns_Friedel_coverage         0.967
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.954
_reflns_number_gt                9875
_reflns_number_total             16199
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt03371a2.cif
_cod_data_source_block           AgPF6_-BTII
_cod_original_cell_volume        1650.8(7)
_cod_original_formula_sum        'C66 H67 Ag F6 N6 O15.50 P'
_cod_database_code               7709864
_shelx_shelxl_version_number     2019/2
_shelx_estimated_absorpt_t_min   0.947
_shelx_estimated_absorpt_t_max   0.979
_shelx_res_checksum              58125
_shelx_hkl_checksum              34447