Kinetic trapping of the host-guest association intermediate and its transformation into a thermodynamic inclusion complex
Oksana Danylyuk; Vladimir P. Fedin; Volodymyr Sashuk; Chemical communications (Cambridge, England) 49 (2013) 1859–1861; doi:10.1039/c3cc37868c

data_7108880
_publ_section_title
;
 Kinetic trapping of the host-guest association intermediate and its
 transformation into a thermodynamic inclusion complex
;
_journal_issue                   18
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              1859
_journal_page_last               1861
_journal_paper_doi               10.1039/c3cc37868c
_journal_volume                  49
_journal_year                    2013
_chemical_absolute_configuration rm
_chemical_formula_sum            'C54 H98 N26 O36'
_chemical_formula_weight         1687.58
_chemical_name_common
'cucurbit(6)uril/neutral adrenaline inclusion complex'
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 102.946(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   12.4610(2)
_cell_length_b                   15.7685(2)
_cell_length_c                   19.4788(3)
_cell_measurement_reflns_used    16101
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      71.313
_cell_measurement_theta_min      3.636
_cell_volume                     3730.13(10)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21b (release 03-02-2012 CrysAlis171 .NET)
(compiled Feb 3 2012,10:37:01)
;
_computing_data_collection
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CrysAlisPro, Agilent Technologies,
Version 1.171.35.21b (release 03-02-2012 CrysAlis171 .NET)
(compiled Feb 3 2012,10:37:01)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21b (release 03-02-2012 CrysAlis171 .NET)
(compiled Feb 3 2012,10:37:01)
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 16.2974
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_source         'SuperNova (Cu) X-ray Source'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0254
_diffrn_reflns_av_sigmaI/netI    0.0271
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            26685
_diffrn_reflns_theta_full        71.45
_diffrn_reflns_theta_max         71.45
_diffrn_reflns_theta_min         3.64
_exptl_absorpt_coefficient_mu    1.082
_exptl_absorpt_correction_T_max  0.8545
_exptl_absorpt_correction_T_min  0.5629
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.463
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1704.8
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.865
_refine_diff_density_min         -0.390
_refine_diff_density_rms         0.085
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.1(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1396
_refine_ls_number_reflns         14194
_refine_ls_number_restraints     1196
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.0859
_refine_ls_R_factor_gt           0.0774
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1817P)^2^+0.6834P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2228
_refine_ls_wR_factor_ref         0.2355
_reflns_number_gt                12198
_reflns_number_total             14194
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            c3cc37868c.txt
_cod_data_source_block           epi_nohcl_new
_cod_original_sg_symbol_H-M      P21
_cod_database_code               7108880