Model Peptide Studies of Ag+ Binding Sites from the Silver Resistance Protein SilE
Chabert, Valentin; Hologne, Maggy; Seneque, Olivier; Crochet, Aurelien; Walker, Olivier; Fromm, Katharina; Chem. Commun.  (2017) –; doi:10.1039/C7CC02630G

data_7120104
_publ_section_title
;
 Model Peptide Studies of Ag+ Binding Sites from the Silver Resistance
 Protein SilE
;
_journal_name_full               'Chem. Commun.'
_journal_paper_doi               10.1039/C7CC02630G
_journal_year                    2017
_chemical_absolute_configuration syn
_chemical_formula_moiety         'C20 H44 Ag2 N4 O8 S4, 2(N O3), 2(H2 O)'
_chemical_formula_sum            'C20 H48 Ag2 N6 O16 S4'
_chemical_formula_weight         972.62
_chemical_name_systematic
'poly(disilver-dimethionine-dinitrate) dihydrate'
_chemical_properties_physical    ', Light-sensitive'
_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'
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2017-05-03 deposited with the CCDC.
2017-05-11 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 99.007(5)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   5.0810(3)
_cell_length_b                   24.7309(12)
_cell_length_c                   14.5097(10)
_cell_measurement_reflns_used    16289
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      25.58
_cell_measurement_theta_min      1.64
_cell_volume                     1800.77(19)
_computing_cell_refinement       'X-Area (Stoe & Cie, 2009)'
_computing_data_collection       'X-Area (Stoe & Cie, 2009)'
_computing_data_reduction        'X-RED32(Stoe & Cie, 2009)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      200(2)
_diffrn_detector_area_resol_mean 6.67
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'STOE IPDS 2'
_diffrn_measurement_method       'rotation method'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_unetI/netI     0.0814
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            6406
_diffrn_reflns_point_group_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        25.189
_diffrn_reflns_theta_max         25.189
_diffrn_reflns_theta_min         1.421
_diffrn_source                   'fine-focus sealed tube'
_diffrn_source_type              'Stoe IPDS2'
_exptl_absorpt_coefficient_mu    1.393
_exptl_absorpt_correction_T_max  0.9681
_exptl_absorpt_correction_T_min  0.7492
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details
;
Stoe & Cie (2002). X-SHAPE. Stoe & Cie, Darmstadt, Germany
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.794
_exptl_crystal_description       needle
_exptl_crystal_F_000             992
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: deuterium oxide'
_exptl_crystal_size_max          0.480
_exptl_crystal_size_mid          0.180
_exptl_crystal_size_min          0.030
_refine_diff_density_max         1.651
_refine_diff_density_min         -1.109
_refine_diff_density_rms         0.192
_refine_ls_abs_structure_details
;
 Flack x determined using 1627 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.02(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.019
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     423
_refine_ls_number_reflns         6406
_refine_ls_number_restraints     59
_refine_ls_restrained_S_all      1.016
_refine_ls_R_factor_all          0.1164
_refine_ls_R_factor_gt           0.0864
_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^)+(0.1193P)^2^+20.4046P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2272
_refine_ls_wR_factor_ref         0.2525
_reflns_Friedel_coverage         0.944
_reflns_Friedel_fraction_full    0.986
_reflns_Friedel_fraction_max     0.986
_reflns_number_gt                4756
_reflns_number_total             6406
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7cc02630g2.cif
_cod_data_source_block           AgMethionine
_cod_database_code               7120104
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.554
_shelx_estimated_absorpt_t_max   0.959
_shelx_res_checksum              13790
_shelx_hkl_checksum              97178