Metal-ion-induced folding and dimerization of a glycoluril decamer in water.
Huang, Wei-Hao; Zavalij, Peter Y.; Isaacs, Lyle; Organic letters 11 (2009) 3918–3921; doi:10.1021/ol901539q

data_1504112
_publ_section_title
;
 Metal-ion-induced folding and dimerization of a glycoluril decamer in
 water.
;
_journal_issue                   17
_journal_name_full               'Organic letters'
_journal_page_first              3918
_journal_page_last               3921
_journal_paper_doi               10.1021/ol901539q
_journal_volume                  11
_journal_year                    2009
_chemical_formula_moiety         'C73 H105.74 F24 N40 Na3.33 O56.53'
_chemical_formula_structural
Na3.33(C57H60N40O20)(C2F3O2)3.33(C2F3O2H)4.67(H2O)20.5
_chemical_formula_sum            'C73 H105.74 F24 N40 Na3.33 O56.53'
_chemical_formula_weight         2980.79
_chemical_name_common
Na3.33(C57H60N40O20)(TFA)3.33(TFAH)4.67(H2O)20.5
_chemical_name_systematic
;
Na3.33(C57H60N40O20)(TFA)3.33(TFAH)4.67(H2O)20.5
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           'SHELXL-97 & ZCIF'
_cell_angle_alpha                90.00
_cell_angle_beta                 124.1850(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   51.867(2)
_cell_length_b                   16.7960(7)
_cell_length_c                   36.2025(15)
_cell_measurement_reflns_used    8972
_cell_measurement_temperature    220(2)
_cell_measurement_theta_max      17.2
_cell_measurement_theta_min      2.3
_cell_volume                     26089.2(19)
_computing_cell_refinement       'SAINT (Bruker, 1999)'
_computing_data_collection       'SMART (Bruker, 1999)'
_computing_data_reduction        SAINT
_computing_molecular_graphics    'XSHEL (Bruker, 1999)'
_computing_publication_material  SHELXL-97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      220(2)
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 8.33
_diffrn_detector_type            'Bruker Smart1000'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details      606,606,606
_diffrn_measurement_device_type  'three-circle diffractometer'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_measurement_specimen_support 'glass capillary'
_diffrn_orient_matrix_type       standard
_diffrn_orient_matrix_UB_11      -0.0032162
_diffrn_orient_matrix_UB_12      -0.0010990
_diffrn_orient_matrix_UB_13      -0.0299426
_diffrn_orient_matrix_UB_21      -0.0230620
_diffrn_orient_matrix_UB_22      0.0027407
_diffrn_orient_matrix_UB_23      -0.0147793
_diffrn_orient_matrix_UB_31      0.0010021
_diffrn_orient_matrix_UB_32      0.0594646
_diffrn_orient_matrix_UB_33      0.0001307
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0654
_diffrn_reflns_av_sigmaI/netI    0.0745
_diffrn_reflns_limit_h_max       49
_diffrn_reflns_limit_h_min       -49
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            58463
_diffrn_reflns_theta_full        20.00
_diffrn_reflns_theta_max         20.00
_diffrn_reflns_theta_min         1.60
_diffrn_source_current           30
_diffrn_source_voltage           50
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    0.158
_exptl_absorpt_correction_T_max  0.974
_exptl_absorpt_correction_T_min  0.837
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.518
_exptl_crystal_description       prism
_exptl_crystal_F_000             13829
_exptl_crystal_id                'Isaacs/WeiHuang compound #3 Na'
_exptl_crystal_size_max          0.46
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.15
_platon_squeeze_details
;
Water and TFA molecules were highly disordered including those 
coordinating sodium and were removed from the structure refinement
(experimental reflection data) using SQUEEZE procedure from Platon
software package.
;
_refine_diff_density_max         0.383
_refine_diff_density_min         -0.215
_refine_diff_density_rms         0.042
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.000
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1101
_refine_ls_number_reflns         12146
_refine_ls_number_restraints     1813
_refine_ls_restrained_S_all      0.978
_refine_ls_R_factor_all          0.1265
_refine_ls_R_factor_gt           0.0799
_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^)+(0.02P)^2^+68.5P], P=(max(Fo^2^,0)+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1607
_refine_ls_wR_factor_ref         0.1723
_reflns_number_gt                5780
_reflns_number_total             12146
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ol901539q_si_002.cif
_cod_data_source_block           1531
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_cell_volume        26089.1(19)
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               1504112
_diffrn_measurement_total_frames-ccd 1818
_diffrn_measurement_frame_width-ccd 0.3
_diffrn_detector_distance-ccd    4.950
_diffrn_measurement_frame_time-ccd 23
_diffrn_measurement_total_time-ccd 15.2
_diffrn_measurement_frame_size-ccd 512