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_7114602
_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            'C124 H116 Ag2 F6 N8 O18 S2'
_chemical_formula_weight         2400.11
_chemical_name_systematic
;
 ?
;
_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                108.091(2)
_cell_angle_beta                 101.907(2)
_cell_angle_gamma                98.189(3)
_cell_formula_units_Z            1
_cell_length_a                   11.7502(4)
_cell_length_b                   15.4683(5)
_cell_length_c                   17.5738(3)
_cell_measurement_reflns_used    22014
_cell_measurement_temperature    100.0(1)
_cell_measurement_theta_max      76.1130
_cell_measurement_theta_min      4.1560
_cell_volume                     2896.75(16)
_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 10.3449
_diffrn_measured_fraction_theta_full 0.999
_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     1.54180
_diffrn_reflns_av_R_equivalents  0.0417
_diffrn_reflns_av_sigmaI/netI    0.0352
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            34617
_diffrn_reflns_theta_full        67.00
_diffrn_reflns_theta_max         76.91
_diffrn_reflns_theta_min         3.33
_diffrn_standards_number         36632
_exptl_absorpt_coefficient_mu    3.708
_exptl_absorpt_correction_T_max  0.752
_exptl_absorpt_correction_T_min  0.672
_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            colorless
_exptl_crystal_density_diffrn    1.376
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rectangular
_exptl_crystal_F_000             1240
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.19
_platon_squeeze_details
;
Disordered solvent methanol molecule that could not be appropriately modeled.
;
_refine_diff_density_max         1.241
_refine_diff_density_min         -1.016
_refine_diff_density_rms         0.090
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.884
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     795
_refine_ls_number_reflns         12033
_refine_ls_number_restraints     140
_refine_ls_restrained_S_all      0.904
_refine_ls_R_factor_all          0.0612
_refine_ls_R_factor_gt           0.0591
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1498P)^2^+3.0028P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1733
_refine_ls_wR_factor_ref         0.1775
_reflns_number_gt                11299
_reflns_number_total             12033
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            c4cc03077j2.cif
_cod_data_source_block           sr1ag_2
_cod_original_cell_volume        2896.75(15)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7114602