Enhancement of Anion Recognition Exhibited by a Halogen-Bonding Rotaxane Host System
Nathan L. Kilah; Matthew D. Wise; Christopher J. Serpell; Amber L. Thompson; Nicholas G. White; Kirsten E. Christensen; Paul D. Beer; Journal of the American Chemical Society 132 (2010) 11893–11895; doi:10.1021/ja105263q

data_4102974
_publ_contact_author             'Paul Beer'
_publ_contact_author_email       paul.beer@chem.ox.ac.uk
_publ_section_title
;
 Enhancement of Anion Recognition Exhibited by a Halogen-Bonding Rotaxane
 Host System
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              11893
_journal_page_last               11895
_journal_paper_doi               10.1021/ja105263q
_journal_volume                  132
_journal_year                    2010
_chemical_formula_moiety         'C81 H97 I N3 O2, C32 H35 N3 O10, Br '
_chemical_formula_sum            'C113 H132 Br I N6 O12'
_chemical_formula_weight         1973.13
_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
_audit_creation_date             10-06-07
_audit_creation_method           CRYSTALS_ver_14.06
_cell_angle_alpha                76.35(5)
_cell_angle_beta                 77.67(5)
_cell_angle_gamma                62.34(4)
_cell_formula_units_Z            2
_cell_length_a                   14.684(4)
_cell_length_b                   14.875(3)
_cell_length_c                   30.286(10)
_cell_measurement_reflns_used    10120
_cell_measurement_temperature    150
_cell_measurement_theta_max      20
_cell_measurement_theta_min      2
_cell_volume                     5652(4)
_computing_cell_refinement
'CrystalClear-SM Expert 2.0 r4 (Rigaku, 2009)'
_computing_data_collection
'CrystalClear-SM Expert 2.0 r4 (Rigaku, 2009)'
_computing_data_reduction
'CrystalClear-SM Expert 2.0 r4 (Rigaku, 2009)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution    'SHELXS 86 (Sheldrick, 1986)'
_diffrn_ambient_temperature      150
_diffrn_detector                 CCD
_diffrn_measured_fraction_theta_full 0.923
_diffrn_measured_fraction_theta_max 0.622
_diffrn_measurement_details
;
scan:
    Number of images: 360
               Slice: -180.0000 - 180.0000
         Image width: 1.0000
            Exp time: 0.5000
       Rotation axis: Phi
               Omega: 0.0000
               Kappa: 0.0000
                 Phi: 0.0000
                 XTD: 60.1556
              2theta: 0.3335

;
_diffrn_measurement_device       'CrystalLogic Kappa (3 circle)'
_diffrn_measurement_device_type  'Rigaku Saturn724+ (2x2 bin mode)'
_diffrn_measurement_method       'profile data from \f-scans'
_diffrn_orient_matrix_type       d*Trek
_diffrn_orient_matrix_UB_11      0.001836
_diffrn_orient_matrix_UB_12      -0.041369
_diffrn_orient_matrix_UB_13      -0.065455
_diffrn_orient_matrix_UB_21      -0.065498
_diffrn_orient_matrix_UB_22      0.037726
_diffrn_orient_matrix_UB_23      0.013964
_diffrn_orient_matrix_UB_31      0.019060
_diffrn_orient_matrix_UB_32      0.026171
_diffrn_orient_matrix_UB_33      -0.011111
_diffrn_radiation_monochromator  Synchrotron
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.68890
_diffrn_reflns_av_R_equivalents  0.181
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            7298
_diffrn_reflns_theta_full        15.064
_diffrn_reflns_theta_max         20.086
_diffrn_reflns_theta_min         1.351
_diffrn_source                   Synchrotron
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.694
_exptl_absorpt_correction_T_max  0.99
_exptl_absorpt_correction_T_min  0.46
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.159
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             2072
_exptl_crystal_size_max          0.067
_exptl_crystal_size_mid          0.007
_exptl_crystal_size_min          0.004
_refine_diff_density_max         0.83
_refine_diff_density_min         -0.63
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.0063
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1713
_refine_ls_number_reflns         6219
_refine_ls_number_restraints     4401
_refine_ls_R_factor_all          0.2130
_refine_ls_R_factor_gt           0.1501
_refine_ls_shift/su_max          0.0037679
_refine_ls_shift/su_mean         0.0002481
_refine_ls_structure_factor_coef Fsqd
_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: 
 0.151E+05 0.242E+05 0.162E+05 0.824E+04 0.266E+04 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.4124
_refine_ls_wR_factor_gt          0.3494
_refine_ls_wR_factor_ref         0.4124
_reflns_limit_h_max              13
_reflns_limit_h_min              -13
_reflns_limit_k_max              14
_reflns_limit_k_min              -11
_reflns_limit_l_max              28
_reflns_limit_l_min              0
_reflns_number_gt                3488
_reflns_number_total             7749
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   7.25
_oxford_diffrn_Wilson_scale      0.04
_oxford_refine_ls_r_factor_ref   0.2130
_oxford_refine_ls_scale          4.8(2)
_oxford_reflns_number_all        6219
_oxford_reflns_threshold_expression_ref I>-3.0\s(I)
_cod_data_source_file            ja105263q_si_005.cif
_cod_data_source_block           7
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_sg_symbol_H-M      'P -1 '
_cod_database_code               4102974