Folding of long-chain alkanediammonium ions promoted by a cucurbituril derivative.
Huang, Wei-Hao; Zavalij, Peter Y.; Isaacs, Lyle; Organic letters 10 (2008) 2577–2580; doi:10.1021/ol800893n

data_1504719
_publ_section_title
;
 Folding of long-chain alkanediammonium ions promoted by a cucurbituril
 derivative.
;
_journal_issue                   12
_journal_name_full               'Organic letters'
_journal_page_first              2577
_journal_page_last               2580
_journal_paper_doi               10.1021/ol800893n
_journal_volume                  10
_journal_year                    2008
_chemical_formula_moiety
'K C86 H84 N48 O28, (C2 F3 O2), (C2 F3 O2 H)6, (H2 O)13'
_chemical_formula_sum            'C100 H116 F21 K N48 O55'
_chemical_formula_weight         3308.51
_chemical_name_common            '[K(H2O)2(CB6')2*2TFAH](TFA)*~4TFAH*~13H2O'
_chemical_name_systematic
;
[K(H2O)2(CB6')2*2TFAH](TFA)*~4TFAH*~13H2O
;
_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                 97.9680(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   31.0746(11)
_cell_length_b                   16.9744(6)
_cell_length_c                   28.0904(10)
_cell_measurement_reflns_used    16943
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      28.0
_cell_measurement_theta_min      2.3
_cell_volume                     14673.9(9)
_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 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details      610,610,610,661
_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      0.0041326
_diffrn_orient_matrix_UB_12      0.0209826
_diffrn_orient_matrix_UB_13      0.0335886
_diffrn_orient_matrix_UB_21      0.0321372
_diffrn_orient_matrix_UB_22      0.0015026
_diffrn_orient_matrix_UB_23      -0.0002562
_diffrn_orient_matrix_UB_31      -0.0024486
_diffrn_orient_matrix_UB_32      0.0550281
_diffrn_orient_matrix_UB_33      -0.0128003
_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  0.0386
_diffrn_reflns_av_sigmaI/netI    0.0322
_diffrn_reflns_limit_h_max       36
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            66732
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.32
_diffrn_source_current           30
_diffrn_source_voltage           50
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    0.166
_exptl_absorpt_correction_T_max  0.984
_exptl_absorpt_correction_T_min  0.917
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.498
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             6800
_exptl_crystal_id                'Isaacs/WeiHuang ?'
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.095
_platon_squeeze_details
;
Void X(av) Y(av) Z(av) Volume  El-Count Vol/Elec Vol/Atom
                 A^3^     (e-)
============================================================
 1  0.045 0.062 -0.002   5740     2720    2.1       17
 
Total (Positive) Electron Count in Voids/Cell =  2720
 
Total (Fo-Fc)map Electron Count in  Unit Cell =  2717
 
VOID-Fo-Fc-Map:    
Rho(min) =     -0.30, Rho(max) =      6.54, RhoCutOff =  0.00

PeaksCloseToAtoms: 
Rho(min) =     -0.68, Rho(max) =      1.23, RhoCutOff =  0.50
 
:: Fo-scale =0.100618E+01 - SinT/L-Min = 0.20 for Fo/Fc-Scaling
 
 
:: Cycle = 13, R(F) = 0.12,          Nref(Hemi) = 25358, 
               R(F > 4SIGF) = 0.08   Nref = 15440
;
_refine_diff_density_max         0.618
_refine_diff_density_min         -0.697
_refine_diff_density_rms         0.052
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.000
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     925
_refine_ls_number_reflns         12908
_refine_ls_number_restraints     256
_refine_ls_restrained_S_all      1.067
_refine_ls_R_factor_all          0.0711
_refine_ls_R_factor_gt           0.0537
_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^)+(0.002P)^2^+46.6P], P=(max(Fo^2^,0)+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1000
_refine_ls_wR_factor_ref         0.1048
_reflns_number_gt                9287
_reflns_number_total             12908
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ol800893n-file004.cif
_cod_data_source_block           1574
_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 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               1504719
_diffrn_measurement_frame_width-ccd 0.3
_diffrn_measurement_total_frames-ccd 2491
_diffrn_measurement_frame_time-ccd 20
_diffrn_measurement_total_time-ccd 18
_diffrn_detector_distance-ccd    5.8
_diffrn_measurement_frame_size-ccd 1024