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_4106109
_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_sum            'C270 H250 Cl30 N24 O24 Ru12'
_chemical_formula_weight         6491.28
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/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                90.00
_cell_angle_beta                 111.009(12)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   43.312(5)
_cell_length_b                   20.595(2)
_cell_length_c                   40.698(4)
_cell_measurement_reflns_used    6201
_cell_measurement_temperature    140(2)
_cell_measurement_theta_max      27.5757
_cell_measurement_theta_min      2.8659
_cell_volume                     33890(7)
_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 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Oxford Diffraction, KM4/Sapphire CCD'
_diffrn_measurement_method       '\w and \p 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  0.1749
_diffrn_reflns_av_sigmaI/netI    0.1477
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            45982
_diffrn_reflns_theta_full        15.86
_diffrn_reflns_theta_max         15.86
_diffrn_reflns_theta_min         2.87
_exptl_absorpt_coefficient_mu    0.809
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.77096
_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    1.272
_exptl_crystal_description       prism
_exptl_crystal_F_000             13072
_exptl_crystal_size_max          0.312
_exptl_crystal_size_mid          0.295
_exptl_crystal_size_min          0.221
_platon_squeeze_details
;
;
_refine_diff_density_max         0.676
_refine_diff_density_min         -0.475
_refine_diff_density_rms         0.128
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.479
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     671
_refine_ls_number_reflns         8029
_refine_ls_number_restraints     1058
_refine_ls_restrained_S_all      1.414
_refine_ls_R_factor_all          0.1857
_refine_ls_R_factor_gt           0.1260
_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^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2857
_refine_ls_wR_factor_ref         0.3008
_reflns_number_gt                4541
_reflns_number_total             8029
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja200580x_si_004.cif
_cod_data_source_block           squeezed
_cod_original_cell_volume        33890(6)
_cod_database_code               4106109