Superior anion induced shuttling behaviour exhibited by a halogen bonding two station rotaxane
Barendt, Timothy A.; Robinson, Sean W.; Beer, Paul D.; Chem. Sci. 7 (2016) 5171–; doi:10.1039/C6SC00783J

data_1543213
_publ_section_title
;
 Superior anion induced shuttling behaviour exhibited by a halogen bonding
 two station rotaxane
;
_journal_issue                   8
_journal_name_full               'Chem. Sci.'
_journal_page_first              5171
_journal_paper_doi               10.1039/C6SC00783J
_journal_volume                  7
_journal_year                    2016
_chemical_compound_source        synthesised
_chemical_formula_moiety
;
2(C109 H113 I N5 O6), 2(C32 H35 N3 O10), C H Cl3, 2(Cl), 2(H2 O)
;
_chemical_formula_sum            'C283 H301 Cl5 I2 N16 O34'
_chemical_formula_weight         4901.46
_chemical_name_common            'Halogen bonding molecular shuttle'
_chemical_name_systematic        'Halogen bonding two-station [2]rotaxane'
_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   difmap
_atom_sites_solution_primary     other
_audit_update_record
;
2016-02-18 deposited with the CCDC.
2016-04-20 downloaded from the CCDC.
;
_cell_angle_alpha                82.872(3)
_cell_angle_beta                 88.588(3)
_cell_angle_gamma                79.909(3)
_cell_formula_units_Z            1
_cell_length_a                   14.8340(5)
_cell_length_b                   16.4316(7)
_cell_length_c                   29.3685(12)
_cell_measurement_reflns_used    11670
_cell_measurement_temperature    100
_cell_measurement_theta_max      25
_cell_measurement_theta_min      2
_cell_volume                     6993.2(5)
_computing_cell_refinement       'CrysAlis, (Oxford Diffraction, 2010)'
_computing_data_collection       'Crystal Clear (Rigaku, 1997--2002)'
_computing_data_reduction        'CrysAlis, (Oxford Diffraction, 2010)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution    'Superflip (Palatinus & Chapuis, 2007)'
_diffrn_ambient_pressure         101
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.878
_diffrn_measured_fraction_theta_max 0.855
_diffrn_measurement_device       Area
_diffrn_measurement_device_type  synchrotron
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  synchrotron
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.68890
_diffrn_reflns_av_R_equivalents  0.295
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            30677
_diffrn_reflns_theta_full        25.117
_diffrn_reflns_theta_max         26.163
_diffrn_reflns_theta_min         1.662
_diffrn_standards_decay_%        -
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.309
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.53
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'CrysAlisPro, (Agilent, 2011)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.164
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             2573.997
_exptl_crystal_preparation       'Molecular machine'
_exptl_crystal_recrystallization_method 'Vapour diffusion'
_exptl_crystal_size_max          0.120
_exptl_crystal_size_mid          0.010
_exptl_crystal_size_min          0.010
_platon_squeeze_details
;
The discrete Fourier transform of the void region were treated as 
contributions to the A and B parts of the calculated structure factors.
;
_refine_diff_density_max         1.09
_refine_diff_density_min         -1.04
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.9710
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1808
_refine_ls_number_reflns         11809
_refine_ls_number_restraints     3001
_refine_ls_R_factor_all          0.1988
_refine_ls_R_factor_gt           0.1389
_refine_ls_shift/su_max          0.0002641
_refine_ls_shift/su_mean         0.0000171
_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: 
 0.401E+04 0.636E+04 0.391E+04 0.160E+04 348. 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.3827
_refine_ls_wR_factor_gt          0.3230
_refine_ls_wR_factor_ref         0.3827
_reflns_limit_h_max              18
_reflns_limit_h_min              -18
_reflns_limit_k_max              20
_reflns_limit_k_min              -20
_reflns_limit_l_max              37
_reflns_limit_l_min              0
_reflns_number_gt                6475
_reflns_number_total             30677
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   5.96
_oxford_diffrn_Wilson_scale      0.41
_oxford_refine_ls_r_factor_ref   0.1988
_oxford_refine_ls_scale          2.09(3)
_oxford_reflns_number_all        11810
_oxford_reflns_threshold_expression_ref I>-3.0\s(I)
_cod_data_source_file            c6sc00783j2.cif
_cod_data_source_block           5Cl
_cod_depositor_comments
;
The following automatic conversions were performed:

'_atom_sites_solution_primary' value 'Other' changed to 'other'
according to
/usr/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

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

Automatic conversion script
Id: cif_fix_values 4268 2015-11-12 08:31:59Z antanas 

 Adding full bibliography for 1543213.cif.
;
_cod_original_cell_volume        6993.2(3)
_cod_original_sg_symbol_H-M      'P -1 '
_cod_database_code               1543213
_platon_squeeze_void_probe_radius 1.20