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_1504113
_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
'Na7, (C57 H60 N40 O20)2, (S O4)2, (C F3 C O2)3, 27(H2 O)'
_chemical_formula_sum            'C120 H174.15 F9 N80 Na7 O81.07 S2'
_chemical_formula_weight         4430.79
_chemical_name_common            7Na(CB5-CH2-CB5)2(SO4)2(TFA)3*27H2O
_chemical_name_systematic
;
7Na(CB5-CH2-CB5)2(SO4)2(TFA)3*27H2O,Z=4
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -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                108.2309(5)
_cell_angle_beta                 99.0790(6)
_cell_angle_gamma                110.5886(5)
_cell_formula_units_Z            4
_cell_length_a                   23.4650(10)
_cell_length_b                   30.5747(13)
_cell_length_c                   31.8174(13)
_cell_measurement_reflns_used    40473
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      25.5
_cell_measurement_theta_min      2.3
_cell_volume                     19353.8(14)
_computing_cell_refinement       Apex2
_computing_data_collection       'Apex2 (Bruker, 2005)'
_computing_data_reduction        Apex2
_computing_molecular_graphics    'XSHEL (Bruker, 2004)'
_computing_publication_material  SHELXL-97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector                 'CCD area detector'
_diffrn_detector_type            'Bruker Smart Apex II'
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_details      610,610,610,318
_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      -0.0314947
_diffrn_orient_matrix_UB_12      -0.0068669
_diffrn_orient_matrix_UB_13      0.0176241
_diffrn_orient_matrix_UB_21      0.0158730
_diffrn_orient_matrix_UB_22      0.0374547
_diffrn_orient_matrix_UB_23      0.0179526
_diffrn_orient_matrix_UB_31      -0.0321774
_diffrn_orient_matrix_UB_32      0.0010318
_diffrn_orient_matrix_UB_33      -0.0239022
_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  0.0379
_diffrn_reflns_av_sigmaI/netI    0.0634
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       36
_diffrn_reflns_limit_k_min       -36
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            158281
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.27
_diffrn_source_current           30
_diffrn_source_voltage           50
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    0.166
_exptl_absorpt_correction_T_max  0.978
_exptl_absorpt_correction_T_min  0.849
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.521
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             9171
_exptl_crystal_id                'Isaacs/WeiHuangCB6 -1 xtal 3'
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.135
_platon_squeeze_details
;
intermolecular are contains about 4 SO4 and 6 CF3COO ions per asymm. unit; 
rest should be water
;
_refine_diff_density_max         0.572
_refine_diff_density_min         -0.323
_refine_diff_density_rms         0.053
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.000
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           fullcycle
_refine_ls_number_parameters     4631
_refine_ls_number_reflns         67869
_refine_ls_number_restraints     24
_refine_ls_restrained_S_all      1.000
_refine_ls_R_factor_all          0.0766
_refine_ls_R_factor_gt           0.0487
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.03P)^2^+11.36P], P=(max(Fo^2^,0)+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1097
_refine_ls_wR_factor_ref         0.1150
_reflns_number_gt                40300
_reflns_number_total             67869
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ol901539q_si_002.cif
_cod_data_source_block           1549
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
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        19353.7(14)
_cod_database_code               1504113