Anion templated assembly of [2]catenanes capable of chloride anion recognition in aqueous solvent media
Evans, Nicholas H.; Allinson, Emma S. H.; Lankshear, Michael D.; Ng, Ka-Yuen; Cowley, Andrew R.; Serpell, Christopher J.; Santos, Sérgio M.; Costa, Paulo J.; Félix, Vítor; Beer, Paul D.; RSC Advances 1 (2011) 995–; doi:10.1039/c1ra00394a

data_7238420
_publ_section_title
;
 Anion templated assembly of [2]catenanes capable of chloride anion
 recognition in aqueous solvent media
;
_journal_issue                   6
_journal_name_full               'RSC Advances'
_journal_page_first              995
_journal_paper_doi               10.1039/c1ra00394a
_journal_volume                  1
_journal_year                    2011
_chemical_formula_moiety         '2(C32 H38 N3 O8), 2Cl'
_chemical_formula_sum            'C64 H76 Cl2 N6 O16'
_chemical_formula_weight         1256.24
_space_group_IT_number           13
_space_group_name_Hall           '-P 2yac'
_space_group_name_H-M_alt        'P 1 2/n 1'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yac'
_symmetry_space_group_name_H-M   'P 1 2/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             11-02-15
_audit_creation_method           CRYSTALS_ver_14.07
_cell_angle_alpha                90
_cell_angle_beta                 95.680(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.303(6)
_cell_length_b                   9.051(3)
_cell_length_c                   43.048(16)
_cell_measurement_reflns_used    12833
_cell_measurement_temperature    150
_cell_measurement_theta_max      32
_cell_measurement_theta_min      1
_cell_volume                     6709(4)
_computing_cell_refinement       'CrystalClear (Rigaku, 1997--2009)'
_computing_data_collection       'CrystalClear (Rigaku, 1997--2009)'
_computing_data_reduction        'CrystalClear (Rigaku, 1997--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    'Superflip (Palatinus & Chapuis, 2007)'
_diffrn_ambient_temperature      150
_diffrn_measured_fraction_theta_full 0.979
_diffrn_measured_fraction_theta_max 0.884
_diffrn_measurement_device       Serial
_diffrn_measurement_device_type  Unknown
_diffrn_measurement_method       \w-scans
_diffrn_radiation_monochromator  'Si(1 1 1) double-crystal monochromator'
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_wavelength     0.68890
_diffrn_reflns_av_R_equivalents  0.163
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       65
_diffrn_reflns_limit_l_min       -65
_diffrn_reflns_number            22082
_diffrn_reflns_theta_full        25.056
_diffrn_reflns_theta_max         31.716
_diffrn_reflns_theta_min         1.277
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.166
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.70
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'CrystalClear (Rigaku, 1997--2009)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.244
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2656
_exptl_crystal_size_max          0.150
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.030
_platon_squeeze_details
;
No satisfactory model could be constructed for the diffuse solvent cavity
and therefore PLATON SQUEEZE was used to account for the electron density
in the refinement.
;
_refine_diff_density_max         1.10
_refine_diff_density_min         -0.71
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.9782
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     793
_refine_ls_number_reflns         8353
_refine_ls_number_restraints     25
_refine_ls_R_factor_all          0.1401
_refine_ls_R_factor_gt           0.1122
_refine_ls_shift/su_max          0.0002607
_refine_ls_shift/su_mean         0.0000277
_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:
66.1 100. 50.0 12.3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.2862
_refine_ls_wR_factor_gt          0.2568
_refine_ls_wR_factor_ref         0.2862
_reflns_limit_h_max              24
_reflns_limit_h_min              -25
_reflns_limit_k_max              13
_reflns_limit_k_min              0
_reflns_limit_l_max              63
_reflns_limit_l_min              0
_reflns_number_gt                6264
_reflns_number_total             22082
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   3.94
_oxford_diffrn_Wilson_scale      49.08
_oxford_refine_ls_r_factor_ref   0.1401
_oxford_refine_ls_scale          0.2608(4)
_oxford_reflns_number_all        8353
_oxford_reflns_threshold_expression_ref I>-3.0\s(I)
_oxford_structure_analysis_title 005CJS11
_cod_data_source_file            c1ra00394a.txt
_cod_data_source_block           BisChlorideCatenane
_cod_original_sg_symbol_H-M      'P 2/n '
_cod_database_code               7238420