Active-template synthesis of “click” [2]rotaxane ligands: self-assembly of mechanically interlocked metallo-supramolecular dimers, macrocycles and oligomers
Noor, Asif; Moratti, Stephen C.; Crowley, James D.; Chem. Sci. 5 (2014) 4283–; doi:10.1039/C4SC01438C

data_1516831
_publ_section_title
;
 Active-template synthesis of &#x201C;click&#x201D; [2]rotaxane ligands:
 self-assembly of mechanically interlocked metallo-supramolecular dimers,
 macrocycles and oligomers
;
_journal_issue                   11
_journal_name_full               'Chem. Sci.'
_journal_page_first              4283
_journal_paper_doi               10.1039/C4SC01438C
_journal_volume                  5
_journal_year                    2014
_chemical_formula_sum            'C44 H32 B2 Cl2 F8 Fe N6'
_chemical_formula_weight         945.13
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.000
_cell_angle_beta                 110.371(5)
_cell_angle_gamma                90.000
_cell_formula_units_Z            4
_cell_length_a                   17.892(5)
_cell_length_b                   14.886(5)
_cell_length_c                   15.952(5)
_cell_measurement_reflns_used    16294
_cell_measurement_temperature    100.0(2)
_cell_measurement_theta_max      76.5110
_cell_measurement_theta_min      4.1850
_cell_volume                     3983(2)
_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, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100.0(2)
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0302
_diffrn_reflns_av_sigmaI/netI    0.0289
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            24933
_diffrn_reflns_theta_full        26.64
_diffrn_reflns_theta_max         26.64
_diffrn_reflns_theta_min         1.83
_exptl_absorpt_coefficient_mu    0.594
_exptl_absorpt_correction_T_max  0.8755
_exptl_absorpt_correction_T_min  0.7928
_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            purple
_exptl_crystal_density_diffrn    1.576
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1920
_exptl_crystal_size_max          0.41
_exptl_crystal_size_mid          0.34
_exptl_crystal_size_min          0.23
_refine_diff_density_max         1.014
_refine_diff_density_min         -0.882
_refine_diff_density_rms         0.080
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.152
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     568
_refine_ls_number_reflns         8281
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.152
_refine_ls_R_factor_all          0.0569
_refine_ls_R_factor_gt           0.0529
_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^)+(0.0427P)^2^+9.8100P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1298
_refine_ls_wR_factor_ref         0.1320
_reflns_number_gt                7667
_reflns_number_total             8281
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4sc01438c2.cif
_cod_data_source_block           tpclfe
_cod_depositor_comments
'Adding full bibliography for 1516829--1516831.cif.'
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               1516831