A redox-active [3]rotaxane capable of binding and electrochemically sensing chloride and sulfate anions
Nicholas H. Evans; Christopher J. Serpell; Paul D. Beer; Chem.Commun. 47 (2011) 8775–; doi:10.1039/c1cc13247d

data_7106731
_publ_section_title
;
 A redox-active [3]rotaxane capable of binding and electrochemically
 sensing chloride and sulfate anions
;
_journal_coden_Cambridge         0182
_journal_name_full               Chem.Commun.
_journal_page_first              8775
_journal_paper_doi               10.1039/c1cc13247d
_journal_volume                  47
_journal_year                    2011
_chemical_formula_moiety
;
C94 H98 Fe N6 O4, 2(C32 H37 N2 O9), 5(C H Cl3), 2(Cl)
;
_chemical_formula_sum            'C163 H177 Cl17 Fe N10 O22'
_chemical_formula_weight         3286.81
_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_method           CRYSTALS_ver_14.07
_cell_angle_alpha                96.343(14)
_cell_angle_beta                 93.555(17)
_cell_angle_gamma                97.116(4)
_cell_formula_units_Z            2
_cell_length_a                   16.141(11)
_cell_length_b                   21.623(15)
_cell_length_c                   24.192(17)
_cell_measurement_reflns_used    0
_cell_measurement_temperature    150
_cell_measurement_theta_max      27
_cell_measurement_theta_min      1
_cell_volume                     8303(10)
_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 0.971
_diffrn_measured_fraction_theta_max 0.836
_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  0.119
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            34946
_diffrn_reflns_theta_full        25.025
_diffrn_reflns_theta_max         28.437
_diffrn_reflns_theta_min         0.956
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.431
_exptl_absorpt_correction_T_max  0.99
_exptl_absorpt_correction_T_min  0.62
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'CrystalClear (Rigaku, 1997--2009)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.315
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             3432
_exptl_crystal_size_max          0.083
_exptl_crystal_size_mid          0.062
_exptl_crystal_size_min          0.013
_platon_squeeze_details
;
?
;
_refine_diff_density_max         1.55
_refine_diff_density_min         -0.90
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.9297
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2051
_refine_ls_number_reflns         19324
_refine_ls_number_restraints     2073
_refine_ls_R_factor_all          0.1720
_refine_ls_R_factor_gt           0.1391
_refine_ls_shift/su_max          0.0017959
_refine_ls_shift/su_mean         0.0000389
_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:
121. 189. 110. 39.9 6.53
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.3271
_refine_ls_wR_factor_gt          0.2982
_refine_ls_wR_factor_ref         0.3271
_reflns_limit_h_max              21
_reflns_limit_h_min              -21
_reflns_limit_k_max              28
_reflns_limit_k_min              -28
_reflns_limit_l_max              30
_reflns_limit_l_min              0
_reflns_number_gt                13759
_reflns_number_total             34946
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   4.12
_oxford_diffrn_Wilson_scale      15.04
_oxford_refine_ls_r_factor_ref   0.1720
_oxford_refine_ls_scale          0.3042(5)
_oxford_reflns_number_all        19324
_oxford_reflns_threshold_expression_ref I>-3.0\s(I)
_oxford_structure_analysis_title 045CJS10
_cod_data_source_file            c1cc13247d.txt
_cod_data_source_block           global
_cod_original_cell_volume        8300(10)
_cod_original_sg_symbol_H-M      'P -1 '
_cod_original_formula_sum        'C163 H177 Cl17 Fe1 N10 O22'
_cod_database_code               7106731