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_4102972
_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         'C21 H33 Cl1 I1 N3'
_chemical_formula_sum            'C21 H33 Cl I N3'
_chemical_formula_weight         489.87
_chemical_name_systematic
;
4-(4-(tert-butyl)phenyl)-5-iodo-3-methyl-1-
n-octyl-1H-1,2,3-triazol-3-ium chloride
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yab'
_symmetry_space_group_name_H-M   'P 1 21/a 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             10-05-10
_audit_creation_method           CRYSTALS_ver_14.07
_cell_angle_alpha                90
_cell_angle_beta                 101.329(11)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.0380(17)
_cell_length_b                   10.9503(17)
_cell_length_c                   15.929(3)
_cell_measurement_reflns_used    3533
_cell_measurement_temperature    150
_cell_measurement_theta_max      26
_cell_measurement_theta_min      1
_cell_volume                     2400.9(7)
_computing_cell_refinement       'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius, 2001).'
_computing_data_reduction        'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'ORTEP3 (Farrugia, 1997)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_diffrn_ambient_temperature      150
_diffrn_measured_fraction_theta_full 0.962
_diffrn_measured_fraction_theta_max 0.942
_diffrn_measurement_device       Area
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.071
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            6984
_diffrn_reflns_theta_full        25.021
_diffrn_reflns_theta_max         26.338
_diffrn_reflns_theta_min         2.848
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.454
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.83
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.355
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1000
_exptl_crystal_size_max          0.37
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.02
_refine_diff_density_max         5.97
_refine_diff_density_min         -1.29
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.1198
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     235
_refine_ls_number_reflns         2328
_refine_ls_number_restraints     95
_refine_ls_R_factor_all          0.1773
_refine_ls_R_factor_gt           0.1482
_refine_ls_shift/su_max          0.0001220
_refine_ls_shift/su_mean         0.0000033
_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: 
 2.36 1.59 1.37 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.2109
_refine_ls_wR_factor_gt          0.1734
_refine_ls_wR_factor_ref         0.1734
_reflns_limit_h_max              17
_reflns_limit_h_min              -17
_reflns_limit_k_max              13
_reflns_limit_k_min              0
_reflns_limit_l_max              19
_reflns_limit_l_min              0
_reflns_number_gt                2328
_reflns_number_total             4613
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   3.55
_oxford_diffrn_Wilson_scale      20.20
_oxford_refine_ls_r_factor_ref   0.1482
_oxford_refine_ls_scale          0.245(2)
_oxford_reflns_number_all        3200
_oxford_reflns_threshold_expression_ref I>2.0\s(I)
_cod_data_source_file            ja105263q_si_003.cif
_cod_data_source_block           2.Cl
_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_cell_volume        2400.8(6)
_cod_original_sg_symbol_Hall     '-P 2yab '
_cod_original_sg_symbol_H-M      'P 1 21/a 1 '
_cod_original_formula_sum        'C21 H33 Cl1 I1 N3'
_cod_database_code               4102972