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_7114600
_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            'C57 H50 Ag F3 N2 O13 S'
_chemical_formula_weight         1167.92
_space_group_IT_number           7
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P -2yac'
_symmetry_space_group_name_H-M   'P 1 n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 91.7631(9)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.04160(10)
_cell_length_b                   21.5483(2)
_cell_length_c                   21.3436(2)
_cell_measurement_reflns_used    26869
_cell_measurement_temperature    100.0(1)
_cell_measurement_theta_max      76.5350
_cell_measurement_theta_min      4.0750
_cell_volume                     5075.83(8)
_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(1)
_diffrn_detector_area_resol_mean 5.1725
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.991
_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           'Cu K\a'
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_R_equivalents  0.0406
_diffrn_reflns_av_sigmaI/netI    0.0460
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            42325
_diffrn_reflns_theta_full        67.00
_diffrn_reflns_theta_max         72.95
_diffrn_reflns_theta_min         4.03
_diffrn_standards_number         42961
_exptl_absorpt_coefficient_mu    4.265
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.57516
_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)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.528
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rectangular
_exptl_crystal_F_000             2400
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.822
_refine_diff_density_min         -0.392
_refine_diff_density_rms         0.069
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.029(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.957
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1391
_refine_ls_number_reflns         16754
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      0.957
_refine_ls_R_factor_all          0.0389
_refine_ls_R_factor_gt           0.0360
_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^)+(0.0573P)^2^+2.5455P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0895
_refine_ls_wR_factor_ref         0.0934
_reflns_number_gt                15923
_reflns_number_total             16754
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            c4cc03077j2.cif
_cod_data_source_block           em2ag
_cod_original_sg_symbol_H-M      Pn
_cod_database_code               7114600