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_4106111
_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            'C238 H292 F2 N28 O34 Ru12'
_chemical_formula_weight         5339.84
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           13
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yac'
_symmetry_space_group_name_H-M   'P 1 2/n 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                 94.407(8)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   25.854(3)
_cell_length_b                   18.338(3)
_cell_length_c                   35.306(5)
_cell_measurement_reflns_used    469
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      22
_cell_measurement_theta_min      3
_cell_volume                     16689(4)
_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_detector_area_resol_mean 8.2812
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker APEX II CCD'
_diffrn_measurement_method       '\w and \p scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1274
_diffrn_reflns_av_sigmaI/netI    0.1218
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       41
_diffrn_reflns_limit_l_min       -41
_diffrn_reflns_number            172853
_diffrn_reflns_theta_full        24.70
_diffrn_reflns_theta_max         24.70
_diffrn_reflns_theta_min         3.01
_exptl_absorpt_coefficient_mu    0.579
_exptl_absorpt_correction_T_max  0.7431
_exptl_absorpt_correction_T_min  0.5731
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2008, Bruker AXS, 2008'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.063
_exptl_crystal_description       prism
_exptl_crystal_F_000             5468
_exptl_crystal_size_max          0.464
_exptl_crystal_size_mid          0.244
_exptl_crystal_size_min          0.128
_platon_squeeze_details
;
;
_refine_diff_density_max         1.724
_refine_diff_density_min         -0.888
_refine_diff_density_rms         0.143
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1293
_refine_ls_number_reflns         28323
_refine_ls_number_restraints     1055
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.1872
_refine_ls_R_factor_gt           0.1109
_refine_ls_shift/su_max          0.061
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1976P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2969
_refine_ls_wR_factor_ref         0.3457
_reflns_number_gt                13634
_reflns_number_total             28323
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja200580x_si_006.cif
_cod_data_source_block           cs069
_cod_database_code               4106111