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_4102973
_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 I2 N3'
_chemical_formula_sum            'C21 H33 I2 N3'
_chemical_formula_weight         581.3208
_chemical_name_systematic
;
4-(4-(tert-butyl)phenyl)-5-iodo-3-methyl-1-
n-octyl-1H-1,2,3-triazol-3-ium iodide
;
_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             10-05-05
_audit_creation_method           CRYSTALS_ver_14.07
_cell_angle_alpha                81.4488(12)
_cell_angle_beta                 80.4591(12)
_cell_angle_gamma                89.9085(16)
_cell_formula_units_Z            4
_cell_length_a                   11.1796(4)
_cell_length_b                   14.7396(5)
_cell_length_c                   15.5956(6)
_cell_measurement_reflns_used    8788
_cell_measurement_temperature    150
_cell_measurement_theta_max      28
_cell_measurement_theta_min      5
_cell_volume                     2505.47(16)
_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    '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_measured_fraction_theta_full 0.981
_diffrn_measured_fraction_theta_max 0.963
_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  0.072
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            11419
_diffrn_reflns_theta_full        25.017
_diffrn_reflns_theta_max         27.797
_diffrn_reflns_theta_min         5.086
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.519
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.65
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.541
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1144
_exptl_crystal_size_max          0.390
_exptl_crystal_size_mid          0.240
_exptl_crystal_size_min          0.020
_refine_diff_density_max         2.19
_refine_diff_density_min         -1.68
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.0630
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     470
_refine_ls_number_reflns         8147
_refine_ls_number_restraints     203
_refine_ls_R_factor_all          0.1062
_refine_ls_R_factor_gt           0.0720
_refine_ls_shift/su_max          0.0004151
_refine_ls_shift/su_mean         0.0000140
_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: 
 2.03 1.17 1.49 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1090
_refine_ls_wR_factor_gt          0.0805
_refine_ls_wR_factor_ref         0.0805
_reflns_limit_h_max              14
_reflns_limit_h_min              -14
_reflns_limit_k_max              19
_reflns_limit_k_min              -18
_reflns_limit_l_max              20
_reflns_limit_l_min              0
_reflns_number_gt                8147
_reflns_number_total             11419
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   2.91
_oxford_diffrn_Wilson_scale      24.60
_oxford_refine_ls_r_factor_ref   0.0720
_oxford_refine_ls_scale          0.2295(5)
_oxford_reflns_number_all        11401
_oxford_reflns_threshold_expression_ref I>2.0\s(I)
_cod_data_source_file            ja105263q_si_004.cif
_cod_data_source_block           2.I
_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_Hall     '-P 1 '
_cod_original_sg_symbol_H-M      'P -1 '
_cod_database_code               4102973