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_4106114
_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         'C120 H126 N12 O12 Ru6, 4(C H Cl3), 2(H2 O)'
_chemical_formula_sum            'C124 H134 Cl12 N12 O14 Ru6'
_chemical_formula_weight         3048.25
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           167
_symmetry_cell_setting           rhombohedral
_symmetry_space_group_name_Hall  '-R 3 2"c'
_symmetry_space_group_name_H-M   'R -3 c :H'
_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                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            6
_cell_length_a                   20.034(3)
_cell_length_b                   20.034(3)
_cell_length_c                   91.487(18)
_cell_measurement_reflns_used    77
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      22
_cell_measurement_theta_min      3
_cell_volume                     31800(9)
_computing_cell_refinement
'Dirax/lsq (Duisenberg & Schreurs, 1989-2000)'
_computing_data_collection       'Collect (Bruker AXS BV, 1997-2004)'
_computing_data_reduction        'EvalCCD (Duisenberg & Schreurs, 1990-2000)'
_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      100(2)
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'Bruker APEX II 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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0725
_diffrn_reflns_limit_h_max       0
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       82
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            2788
_diffrn_reflns_theta_full        18.90
_diffrn_reflns_theta_max         18.90
_diffrn_reflns_theta_min         3.11
_exptl_absorpt_coefficient_mu    0.607
_exptl_absorpt_correction_T_max  0.6996
_exptl_absorpt_correction_T_min  0.3000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2008, Bruker AXS, 2008'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    0.955
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             9252
_exptl_crystal_size_max          0.59
_exptl_crystal_size_mid          0.38
_exptl_crystal_size_min          0.30
_platon_squeeze_details
;
;
_refine_diff_density_max         1.437
_refine_diff_density_min         -0.589
_refine_diff_density_rms         0.142
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.278
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     253
_refine_ls_number_reflns         2788
_refine_ls_number_restraints     108
_refine_ls_restrained_S_all      1.274
_refine_ls_R_factor_all          0.1870
_refine_ls_R_factor_gt           0.1375
_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^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3449
_refine_ls_wR_factor_ref         0.3832
_reflns_number_gt                1387
_reflns_number_total             2788
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja200580x_si_009.cif
_cod_data_source_block           cs039
_cod_original_cell_volume        31801(9)
_cod_original_sg_symbol_H-M      'R -3 c'
_cod_database_code               4106114