Binding modes of methyl α-d-glucopyranoside to an artificial receptor in crystalline complexes
Köhler, Linda; Hübler, Conrad; Seichter, Wilhelm; Mazik, Monika; RSC Advances 11 (2021) 22221–22229; doi:10.1039/D1RA03390E

data_7243107
_publ_section_title
;
 Binding modes of methyl \a-d-glucopyranoside to an artificial receptor in
 crystalline complexes
;
_journal_issue                   36
_journal_name_full               'RSC Advances'
_journal_page_first              22221
_journal_page_last               22229
_journal_paper_doi               10.1039/D1RA03390E
_journal_volume                  11
_journal_year                    2021
_chemical_absolute_configuration rm
_chemical_formula_moiety         'C33 H45 N9, C7 H14 O6, 3(C H4 O), 0.5(H2 O)'
_chemical_formula_sum            'C43 H72 N9 O9.5'
_chemical_formula_weight         867.09
_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   mixed
_audit_block_doi                 10.5517/ccdc.csd.cc27ktyl
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2021-03-24 deposited with the CCDC.	2021-06-01 downloaded from the CCDC.
;
_cell_angle_alpha                67.762(9)
_cell_angle_beta                 86.941(9)
_cell_angle_gamma                84.111(9)
_cell_formula_units_Z            2
_cell_length_a                   12.2116(14)
_cell_length_b                   14.5632(16)
_cell_length_c                   14.5319(17)
_cell_measurement_reflns_used    10270
_cell_measurement_temperature    113(2)
_cell_measurement_theta_max      25.96
_cell_measurement_theta_min      2.48
_cell_volume                     2379.2(5)
_computing_cell_refinement       'STOE X-AREA (Stoe & Cie, 2002)'
_computing_data_collection       'STOE X-AREA (Stoe & Cie, 2002)'
_computing_data_reduction        'STOE X-RED (Stoe & Cie, 2002)'
_computing_molecular_graphics    'ORTEP-3 (Farrugia, 2012)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      113(2)
_diffrn_detector                 'image plate (34 cm diameter)'
_diffrn_detector_area_resol_mean 6.67
_diffrn_detector_type            STOE
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_details      ' 976 frames, detector distance = 130 mm'
_diffrn_measurement_device       '2-circle goniometer'
_diffrn_measurement_device_type  'STOE IPDS 2T'
_diffrn_measurement_method       'rotation method'
_diffrn_radiation_collimation    '0.5 mm diameter, monocapillary'
_diffrn_radiation_monochromator  'plane graphite'
_diffrn_radiation_polarisn_norm  0
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0189
_diffrn_reflns_av_unetI/netI     0.0150
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            73592
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.711
_diffrn_reflns_theta_min         2.833
_diffrn_source
'sealed X-ray tube, 12 x 0.4 mm long-fine focus'
_diffrn_source_current           40
_diffrn_source_power             2.000
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    0.086
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.210
_exptl_crystal_description       irrgular
_exptl_crystal_F_000             938
_exptl_crystal_size_max          0.420
_exptl_crystal_size_mid          0.380
_exptl_crystal_size_min          0.320
_refine_diff_density_max         0.579
_refine_diff_density_min         -0.562
_refine_diff_density_rms         0.063
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1186
_refine_ls_number_reflns         17273
_refine_ls_number_restraints     22
_refine_ls_restrained_S_all      1.071
_refine_ls_R_factor_all          0.0590
_refine_ls_R_factor_gt           0.0536
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0983P)^2^+1.3935P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1476
_refine_ls_wR_factor_ref         0.1553
_reflns_Friedel_coverage         1.000
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.989
_reflns_number_gt                16001
_reflns_number_total             17273
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1ra03390e2.cif
_cod_data_source_block           Likoe27bnew1
_cod_depositor_comments
;

2024-12-16
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C86 H144 N18 O19'
_cod_original_formula_weight         1734.18
_cod_original_formula_moiety
'2(C33 H45 N9), 2(C7 H14 O6), 6(C H4 O), H2 O'
_cod_original_formula_units_Z            1
_cod_database_code               7243107
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.965
_shelx_estimated_absorpt_t_max   0.973
_iucr_geom_hbonds_special_details
;
Cg1 represents the centroid of the C1-C6 ring;
Cg2 represents the centroid of the C8-C11/N2/N3;
Cg3 represents the centroid of the C17-C20/N5/N6;
Cg4 represents the centroid of the C26-C29/N8/N9;
Cg1' represents the centroid of the C1A-C16A ring;
Cg2' represents the centroid of the C8A-C11A/N2A/N3A;
Cg4' represents the centroid of the C26A-C29A/N8A/N9A
;
_shelx_res_checksum              3097