Noncovalent Interactions within a Synthetic Receptor Can Reinforce Guest Binding
Zaida Rodriguez-Docampo; Sofia I. Pascu; Stefan Kubik; Sijbren Otto; Journal of the American Chemical Society 128 (2006) 11206–11210; doi:10.1021/ja062389h

data_4110837
_publ_section_title
;
 Noncovalent Interactions within a Synthetic Receptor Can Reinforce Guest
 Binding
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              11206
_journal_page_last               11210
_journal_paper_doi               10.1021/ja062389h
_journal_volume                  128
_journal_year                    2006
_chemical_absolute_configuration syn
_chemical_compound_source
;
synthesis as described
;
_chemical_formula_moiety
;
C69 H70 N18 O13 S4, C16 H36 N, C16 H36 N, O4 S, H2 O
;
_chemical_formula_sum            'C101 H144 N20 O18 S5'
_chemical_formula_weight         2086.66
_chemical_name_systematic        ?
_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
_audit_creation_date             04-05-28
_audit_creation_method           CRYSTALS_ver_12.20
_cell_angle_alpha                90
_cell_angle_beta                 93.196(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   12.9731(10)
_cell_length_b                   16.0397(10)
_cell_length_c                   26.4260(10)
_cell_measurement_reflns_used    13502
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      22.28
_cell_measurement_theta_min      2.18
_cell_volume                     5490.3(6)
_computing_cell_refinement       'Bruker SAINT (Bruker AXS, 1994)'
_computing_data_collection       'Bruker SMART (Bruker AXS, 1994)'
_computing_data_reduction        'Bruker SAINT (Bruker AXS, 1994)'
_computing_molecular_graphics
; 
 CAMERON (Watkin et al 1996) 
;
_computing_publication_material
; 
 CRYSTALS (Watkin et al 2001) 
;
_computing_structure_refinement
; 
 CRYSTALS (Watkin et al 2001) 
;
_computing_structure_solution    'SHELXTL v6.12 (Bruker AXS, 2001)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker SMART CCD'
_diffrn_measurement_method       'Thin slice \w-scans'
_diffrn_radiation_monochromator  'Silicon 111'
_diffrn_radiation_source         'Daresbury SRS, Station 9.8'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.6923
_diffrn_reflns_av_R_equivalents  0.04
_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       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            35394
_diffrn_reflns_theta_full        23.346
_diffrn_reflns_theta_max         23.346
_diffrn_reflns_theta_min         1.712
_diffrn_standards_decay_%        0.00
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.178
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  1.00
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 
  Correction applied by SADABS - note that the transmission factors are
  not real since they include corrections for beam decay and possibly
  crystal decay (the two cannot be distinguished).
  The numbers listed in the CIF are those calculated by CRYSTALS.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.261
_exptl_crystal_description       block
_exptl_crystal_F_000             2223.000
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.35
_refine_diff_density_min         -0.95
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.1570
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     979
_refine_ls_number_reflns         5124
_refine_ls_number_restraints     344
_refine_ls_R_factor_all          0.1431
_refine_ls_R_factor_gt           0.1128
_refine_ls_shift/su_max          0.013418
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details
;
 Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) 
 [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] 
 where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax 
 Method = Robust Weighting (Prince, 1982) 
 W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ 
 A~i~ are: 
 1.13 1.35 0.484 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1534
_refine_ls_wR_factor_gt          0.1248
_refine_ls_wR_factor_ref         0.1248
_reflns_limit_h_max              14
_reflns_limit_h_min              -14
_reflns_limit_k_max              17
_reflns_limit_k_min              0
_reflns_limit_l_max              29
_reflns_limit_l_min              0
_reflns_number_gt                5124
_reflns_number_total             8281
_reflns_threshold_expression     I>2.00u(I)
_cod_data_source_file            ja062389hsi20060407_070730.cif
_cod_data_source_block           cam162
_cod_depositor_comments
;
 Changing the '_atom_type_symbol' data item values to match those of the
 '_atom_site_type_symbol' data item.

 Antanas Vaitkus,
 2017-09-27

 Correcting the way attached hydrogen atoms are marked for atoms 'O500' and
 'O501' by changing the number of attached hydrogens to '1' for each of the
 atoms. The atoms were previously marked as having '0.651' and '0.349' attached
 hydrogens respectively to reflect the partial occupancy of the atoms themselves.

 Antanas Vaitkus,
 2017-09-27
;
_cod_original_sg_symbol_H-M      'P 1 21 1 '
_cod_original_formula_sum        ' C101 H144 N20 O18.00 S5.00 '
_cod_database_code               4110837