A guanidino-γ-cyclodextrin superdimer generates a twin receptor for phosphate dimers assembled by anti-electrostatic hydrogen bonds
Saridakis, Emmanuel; Kasimati, Eleni Marina; Yannakopoulou, Konstantina; Mavridis, Irene M.; Chemical Communications  (2022) –; doi:10.1039/D2CC00323F

data_7129917
_publ_section_title
;
 A guanidino-\g-cyclodextrin superdimer generates a twin receptor for
 phosphate dimers assembled by anti-electrostatic hydrogen bonds
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/D2CC00323F
_journal_year                    2022
_chemical_formula_moiety
'2(C56 H104 N24 O32), 7(H O4 P), H4N, 12.32(H2O) 2[H O4 P] [H4N]'
_chemical_formula_sum            'C112 H249.64 N50 O112.32 P9'
_chemical_formula_weight         4373.09
_chemical_name_common
;
Perguanidino-gamma-Cyclodextrin
;
_chemical_name_systematic
;
Perguanidino-gamma-Cyclodextrin
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           20
_space_group_name_Hall           'C 2c 2'
_space_group_name_H-M_alt        'C 2 2 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2022-03-31 deposited with the CCDC.	2022-04-01 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   26.90(2)
_cell_length_b                   36.40(2)
_cell_length_c                   53.20(2)
_cell_measurement_reflns_used    19490
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      24.490
_cell_measurement_theta_min      8.747
_cell_volume                     52091(5)
_computing_cell_refinement
;
XDS (Kabsch, W. XDS. Acta Crystallog, 2010, D66, 125
;
_computing_data_collection
;
proprietary software and Mosflm (Leslie, 1990)
;
_computing_data_reduction
;
XDS (Kabsch, W. XDS. Acta Crystallog, 2010, D66, 125
;
_computing_molecular_graphics
;
Delano, W. L. The PyMOL Molecular Graphics System. 
DeLano Scientific LLC: San Carlos, CA, 2002 
;
_computing_publication_material
;
Pymol (DeLano, 2002) and Mercury (Macrae et al, 2020)
;
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution
;
SHELXD (Sheldrick G.M.,Acta Crystallog, 2010, D66,479
;
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.944
_diffrn_measured_fraction_theta_max 0.944
_diffrn_measurement_device_type  CCD
_diffrn_measurement_method       oscillation
_diffrn_radiation_type           SYNCHROTRON
_diffrn_radiation_wavelength     0.912
_diffrn_reflns_av_R_equivalents  0.0624
_diffrn_reflns_av_unetI/netI     0.0352
_diffrn_reflns_Laue_measured_fraction_full 0.944
_diffrn_reflns_Laue_measured_fraction_max 0.944
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       48
_diffrn_reflns_limit_l_min       -48
_diffrn_reflns_number            108839
_diffrn_reflns_point_group_measured_fraction_full 0.949
_diffrn_reflns_point_group_measured_fraction_max 0.949
_diffrn_reflns_theta_full        24.490
_diffrn_reflns_theta_max         24.490
_diffrn_reflns_theta_min         8.747
_diffrn_source                   'DARESBURY RADIATION SOURCE'
_exptl_absorpt_coefficient_mu    0.289
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.115
_exptl_crystal_density_method    none
_exptl_crystal_description       diamond-shaped
_exptl_crystal_F_000             17447
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.201
_refine_diff_density_min         -0.132
_refine_diff_density_rms         0.033
_refine_ls_abs_structure_details
;
 Flack x determined using 5736 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.25(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   2.386
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2706
_refine_ls_number_reflns         19490
_refine_ls_number_restraints     1274
_refine_ls_restrained_S_all      2.376
_refine_ls_R_factor_all          0.1397
_refine_ls_R_factor_gt           0.1290
_refine_ls_shift/su_max          0.054
_refine_ls_shift/su_mean         0.006
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3187
_refine_ls_wR_factor_ref         0.3299
_reflns_Friedel_coverage         0.883
_reflns_Friedel_fraction_full    0.955
_reflns_Friedel_fraction_max     0.955
_reflns_number_gt                15727
_reflns_number_total             19490
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2cc00323f2.cif
_cod_data_source_block           shelxl
_cod_original_cell_volume        52091(52)
_cod_database_code               7129917
_shelx_shelxl_version_number     2018/3
_shelx_res_checksum              22683
_shelx_hkl_checksum              12192