Wetting the lock and key enthalpically favours polyelectrolytes binding
Jeamet, Emeric; Septavaux, Jean; Héloin, Alexandre; Donnier-Maréchal, Marion; Dumartin, Melissa; OURRI, Benjamin; Mandal, Pradeep Kumar; Huc, Ivan; Bignon, Emmanuelle; Dumont, Elise; Morell, Christophe; Francoia, Jean-Patrick; PERRET, Florent; Vial, Laurent; Leclaire, Julien; Chemical Science  (2018) –; doi:10.1039/C8SC02966K

data_1550019
_publ_section_title
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 Wetting the lock and key enthalpically favours polyelectrolytes binding
;
_journal_name_full               'Chemical Science'
_journal_paper_doi               10.1039/C8SC02966K
_journal_year                    2018
_chemical_formula_moiety         'C32 H8 O16 S8, 9(O), C6 H14 N3 O'
_chemical_formula_sum            'C38 H23 N3 O26 S8'
_chemical_formula_weight         1194.07
_chemical_name_common            A4
_chemical_properties_physical
', Air-sensitive,Moisture-sensitive,Heat-sensitive'
_space_group_crystal_system      monoclinic
_space_group_IT_number           7
_space_group_name_Hall           'P -2yac'
_space_group_name_H-M_alt        'P 1 n 1'
_symmetry_space_group_name_Hall  'P -2yac'
_symmetry_space_group_name_H-M   'P 1 n 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2017-04-21
_audit_creation_method
;
Olex2 1.2
(compiled 2016.11.30 svn.r3356 for OlexSys, GUI svn.r5269)
;
_audit_update_record
;
2017-06-07 deposited with the CCDC.
2018-10-08 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 91.8620(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   11.05830(10)
_cell_length_b                   10.71380(10)
_cell_length_c                   21.6433(3)
_cell_measurement_reflns_used    30597
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      73.257
_cell_measurement_theta_min      4.055
_cell_volume                     2562.87(5)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_device_type  'Rigaku PILATUS 200K'
_diffrn_measurement_method       \w-scans
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0343
_diffrn_reflns_av_unetI/netI     0.0214
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.984
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            35906
_diffrn_reflns_point_group_measured_fraction_full 0.839
_diffrn_reflns_point_group_measured_fraction_max 0.822
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.983
_diffrn_reflns_theta_min         4.087
_diffrn_source                   'Rigaku FRX'
_exptl_absorpt_coefficient_mu    4.028
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.81885
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.547
_exptl_crystal_description       prism
_exptl_crystal_F_000             1216
_exptl_crystal_recrystallization_method 'vapour diffusion'
_exptl_crystal_size_max          0.07
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.674
_refine_diff_density_min         -0.462
_refine_diff_density_rms         0.111
_refine_ls_abs_structure_details
;
 Flack x determined using 3092 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.420(16)
_refine_ls_extinction_coef       0.0008(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2016/4 (Sheldrick 2016)'
_refine_ls_goodness_of_fit_ref   0.987
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     661
_refine_ls_number_reflns         8551
_refine_ls_number_restraints     31
_refine_ls_restrained_S_all      0.985
_refine_ls_R_factor_all          0.0655
_refine_ls_R_factor_gt           0.0633
_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^)+(0.1170P)^2^+8.6284P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1758
_refine_ls_wR_factor_ref         0.1818
_reflns_Friedel_coverage         0.668
_reflns_Friedel_fraction_full    0.679
_reflns_Friedel_fraction_max     0.659
_reflns_number_gt                8327
_reflns_number_total             8551
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8sc02966k2.cif
_cod_data_source_block           A4_L_D_LysNH2
_cod_database_code               1550019
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H,H) groups
2. Restrained distances
 O6B-C4B
 1.28 with sigma of 0.02
 O5B-C4B
 1.24 with sigma of 0.02
 O4B-C2B
 1.24 with sigma of 0.02
 O13B-C7B
 1.24 with sigma of 0.02
 O14B-C7B
 1.28 with sigma of 0.02
 O12B-C6B
 1.24 with sigma of 0.02
 O11B-C6B
 1.28 with sigma of 0.02
 O3B-C2B
 1.28 with sigma of 0.02
 O15B-C8B
 1.24 with sigma of 0.02
 O16B-C8B
 1.28 with sigma of 0.02
 O7B-C3B
 1.24 with sigma of 0.02
 O8B-C3B
 1.28 with sigma of 0.02
 O9B-C5B
 1.24 with sigma of 0.02
 O10B-C5B
 1.28 with sigma of 0.02
 O2B-C1B
 1.28 with sigma of 0.02
 O1B-C1B
 1.24 with sigma of 0.02
 O1-C021
 1.24 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(N1L) \\sim Ueq, Uanis(O1W) \\sim Ueq: with sigma of 0.1 and sigma for
terminal atoms of 0.2
4. Others
 Fixed Sof: N1L(0.75) H1LA(0.75) H1LB(0.75) N1(0.25) H1B(0.25) H1C(0.25)
5.a Secondary CH2 refined with riding coordinates:
 C01J(H01C,H01D), C01O(H01E,H01F), C01R(H01G,H01H), C020(H02A,H02B)
5.b Aromatic/amide H refined with riding coordinates:
 C9A(H9A)
5.c Fitted hexagon refined as free rotating group:
 C6A(C1A,C2A,C3A,C4A,C5A), C10A(C11A,C12A,C7A,C8A,C9A), C16A(C17A,C18A,C13A,
 C14A,C15A), C19A(C20A,C21A,C22A,C23A,C24A)
5.d X=CH2 refined with riding coordinates:
 N1L(H1LA,H1LB), N1(H1B,H1C), N1W(H1WA,H1WB), N011(H01A,H01B)
;
_shelx_res_checksum              6671
_shelx_shelxl_version_number     2016/4
_olex2_submission_special_instructions 'No special instructions were received'