Connection of Metallamacrocycles via Dynamic Covalent Chemistry: A Versatile Method for the Synthesis of Molecular Cages
Anton Granzhan; Clément Schouwey; Thomas Riis-Johannessen; Rosario Scopelliti; Kay Severin; Journal of the American Chemical Society 133 (2011) 7106–7115; doi:10.1021/ja200580x

data_4106108
_publ_section_title
;
 Connection of Metallamacrocycles via Dynamic Covalent Chemistry: A
 Versatile Method for the Synthesis of Molecular Cages
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              7106
_journal_page_last               7115
_journal_paper_doi               10.1021/ja200580x
_journal_volume                  133
_journal_year                    2011
_chemical_formula_moiety         'C63 H57 N3 O9 Ru3, C H Cl3'
_chemical_formula_sum            'C64 H58 Cl3 N3 O9 Ru3'
_chemical_formula_weight         1422.69
_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                93.476(4)
_cell_angle_beta                 96.109(4)
_cell_angle_gamma                114.941(5)
_cell_formula_units_Z            2
_cell_length_a                   11.7185(6)
_cell_length_b                   13.5985(8)
_cell_length_c                   21.1648(8)
_cell_measurement_reflns_used    16268
_cell_measurement_temperature    140(2)
_cell_measurement_theta_max      28.6450
_cell_measurement_theta_min      2.9180
_cell_volume                     3019.9(3)
_computing_cell_refinement
; 
CrysAlisPro, Oxford Diffraction Ltd., 
Version 1.171.33.66 (release 28-04-2010 CrysAlis171 .NET) 
(compiled Apr 28 2010,14:27:37) 
;
_computing_data_collection
; 
CrysAlisPro, Oxford Diffraction Ltd., 
Version 1.171.33.66 (release 28-04-2010 CrysAlis171 .NET) 
(compiled Apr 28 2010,14:27:37) 
;
_computing_data_reduction
; 
CrysAlisPro, Oxford Diffraction Ltd., 
Version 1.171.33.66 (release 28-04-2010 CrysAlis171 .NET) 
(compiled Apr 28 2010,14:27:37) 
;
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      140(2)
_diffrn_detector_area_resol_mean 8.2812
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device_type  'Oxford Diffraction, KM4/Sapphire CCD'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0198
_diffrn_reflns_av_sigmaI/netI    0.0194
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            26161
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         2.92
_exptl_absorpt_coefficient_mu    0.932
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.83428
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
CrysAlisPro, Oxford Diffraction Ltd., 
Version 1.171.33.66 (release 28-04-2010 CrysAlis171 .NET) 
(compiled Apr 28 2010,14:27:37) 
empirical absorption correction using spherical harmonics, 
 implemented in SCALE3 ABSPACK scaling algorithm. 
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.565
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             1436
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.17
_platon_squeeze_details          ' '
_refine_diff_density_max         0.988
_refine_diff_density_min         -0.619
_refine_diff_density_rms         0.086
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     776
_refine_ls_number_reflns         13645
_refine_ls_number_restraints     30
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.0339
_refine_ls_R_factor_gt           0.0303
_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^)+(0.0578P)^2^+1.9543P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0864
_refine_ls_wR_factor_ref         0.0885
_reflns_number_gt                12223
_reflns_number_total             13645
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja200580x_si_003.cif
_cod_data_source_block           agxi36a
_cod_database_code               4106108