CuAAC 'click' active-template synthesis of functionalised [2]rotaxanes using small exo-substituted macrocycles: how small is too small?
Asif Noor; Warrick K. C. Lo; Stephen C. Moratti; James D. Crowley; Chem.Commun. 50 (2014) 7044–; doi:10.1039/C4CC03077J

data_7114601
_publ_section_title
;
 CuAAC 'click' active-template synthesis of functionalised [2]rotaxanes
 using small exo-substituted macrocycles: how small is too small?
;
_journal_name_full               Chem.Commun.
_journal_page_first              7044
_journal_paper_doi               10.1039/C4CC03077J
_journal_volume                  50
_journal_year                    2014
_chemical_formula_sum            'C61 H58 Ag F3 N2 O13 S'
_chemical_formula_weight         1224.02
_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
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                106.432(2)
_cell_angle_beta                 90.948(2)
_cell_angle_gamma                108.504(2)
_cell_formula_units_Z            2
_cell_length_a                   12.3931(3)
_cell_length_b                   12.7490(3)
_cell_length_c                   19.1316(2)
_cell_measurement_reflns_used    30283
_cell_measurement_temperature    100.0(2)
_cell_measurement_theta_max      76.4710
_cell_measurement_theta_min      3.7650
_cell_volume                     2730.58(11)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR97 (Altomare et al., 1997)'
_diffrn_ambient_temperature      100.0(2)
_diffrn_detector_area_resol_mean 10.3449
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_source         'SuperNova (Cu) X-ray Source'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_R_equivalents  0.0415
_diffrn_reflns_av_sigmaI/netI    0.0257
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            41324
_diffrn_reflns_theta_full        67.00
_diffrn_reflns_theta_max         77.32
_diffrn_reflns_theta_min         3.79
_diffrn_standards_number         44865
_exptl_absorpt_coefficient_mu    3.991
_exptl_absorpt_correction_T_max  0.559
_exptl_absorpt_correction_T_min  0.395
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
Analytical numeric absorption correction using a multifaceted crystal
            model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.489
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       triangular
_exptl_crystal_F_000             1264
_exptl_crystal_size_max          0.44
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.23
_refine_diff_density_max         0.670
_refine_diff_density_min         -1.341
_refine_diff_density_rms         0.086
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     735
_refine_ls_number_reflns         11399
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0423
_refine_ls_R_factor_gt           0.0416
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0751P)^2^+1.8781P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1133
_refine_ls_wR_factor_ref         0.1142
_reflns_number_gt                11104
_reflns_number_total             11399
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            c4cc03077j2.cif
_cod_data_source_block           em3ag
_cod_original_cell_volume        2730.58(10)
_cod_database_code               7114601