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_4106107
_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         'C66 H63 N3 O9 Ru3,  1.6(C H Cl3)'
_chemical_formula_sum            'C67.6 H64.6 Cl4.8 N3 O9 Ru3'
_chemical_formula_weight         1536.39
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
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_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                104.466(7)
_cell_angle_beta                 92.224(6)
_cell_angle_gamma                111.419(8)
_cell_formula_units_Z            2
_cell_length_a                   12.8074(10)
_cell_length_b                   17.1174(15)
_cell_length_c                   19.0333(13)
_cell_measurement_reflns_used    9064
_cell_measurement_temperature    140(2)
_cell_measurement_theta_max      27.5528
_cell_measurement_theta_min      2.8799
_cell_volume                     3722.0(6)
_computing_cell_refinement
; 
CrysAlisPro, Oxford Diffraction Ltd., 
Version 1.171.33.41 (release 06-05-2009 CrysAlis171 .NET) 
(compiled May  6 2009,17:20:42) 
;
_computing_data_collection
; 
CrysAlisPro, Oxford Diffraction Ltd., 
Version 1.171.33.41 (release 06-05-2009 CrysAlis171 .NET) 
(compiled May  6 2009,17:20:42) 
;
_computing_data_reduction
; 
CrysAlisPro, Oxford Diffraction Ltd., 
Version 1.171.33.41 (release 06-05-2009 CrysAlis171 .NET) 
(compiled May  6 2009,17:20:42) 
;
_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 0.988
_diffrn_measured_fraction_theta_max 0.988
_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  0.0567
_diffrn_reflns_av_sigmaI/netI    0.1049
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            27081
_diffrn_reflns_theta_full        25.68
_diffrn_reflns_theta_max         25.68
_diffrn_reflns_theta_min         2.91
_exptl_absorpt_coefficient_mu    0.824
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.74871
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
CrysAlisPro, Oxford Diffraction Ltd., 
Version 1.171.33.41 (release 06-05-2009 CrysAlis171 .NET) 
(compiled May  6 2009,17:20:42) 
empirical absorption correction using spherical harmonics, 
 implemented in SCALE3 ABSPACK scaling algorithm. 
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.371
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1554
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.34
_exptl_crystal_size_min          0.25
_platon_squeeze_details
;
;
_refine_diff_density_max         2.772
_refine_diff_density_min         -1.371
_refine_diff_density_rms         0.226
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     820
_refine_ls_number_reflns         13965
_refine_ls_number_restraints     66
_refine_ls_restrained_S_all      1.067
_refine_ls_R_factor_all          0.1507
_refine_ls_R_factor_gt           0.1015
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1917P)^2^+8.0279P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2896
_refine_ls_wR_factor_ref         0.3137
_reflns_number_gt                8335
_reflns_number_total             13965
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja200580x_si_002.cif
_cod_data_source_block           ag-xi-06
_cod_original_cell_volume        3722.0(5)
_cod_original_formula_sum        'C67.60 H64.60 Cl4.80 N3 O9 Ru3'
_cod_database_code               4106107