Metal-organic frameworks with dynamic interlocked components.
Vukotic, V. Nicholas; Harris, Kristopher J.; Zhu, Kelong; Schurko, Robert W.; Loeb, Stephen J.; Nature chemistry 4 (2012) 456–460; doi:10.1038/nchem.1354

data_1508205
_publ_section_title
;
 Metal-organic frameworks with dynamic interlocked components.
;
_journal_issue                   6
_journal_name_full               'Nature chemistry'
_journal_page_first              456
_journal_page_last               460
_journal_paper_doi               10.1038/nchem.1354
_journal_volume                  4
_journal_year                    2012
_chemical_formula_sum            'C35 H55 Cu2 N O19'
_chemical_formula_weight         920.88
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           148
_symmetry_cell_setting           hexagonal
_symmetry_space_group_name_Hall  '-R 3'
_symmetry_space_group_name_H-M   'R -3 :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            9
_cell_length_a                   23.127(4)
_cell_length_b                   23.127(4)
_cell_length_c                   19.723(3)
_cell_measurement_reflns_used    368
_cell_measurement_temperature    148(2)
_cell_measurement_theta_max      24.99
_cell_measurement_theta_min      1.76
_cell_volume                     9136(3)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL XPREP'
_computing_molecular_graphics    'Bruker SHELXTL XP'
_computing_publication_material  'Bruker SHELXTL XCIF'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      148(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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  0.0834
_diffrn_reflns_av_sigmaI/netI    0.0654
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            28250
_diffrn_reflns_theta_full        24.99
_diffrn_reflns_theta_max         24.99
_diffrn_reflns_theta_min         1.76
_exptl_absorpt_coefficient_mu    1.126
_exptl_absorpt_correction_T_max  0.8185
_exptl_absorpt_correction_T_min  0.5623
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.506
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             4338
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.34
_exptl_crystal_size_min          0.28
_platon_squeeze_details
;
 The unit cell contains an estimated 27 molecules of water which have
 been treated as a diffuse contribution to the overall scattering 
 without specific atom positions by SQUEEZE/PLATON.
 
 Refinement of F^2^ against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F^2^, conventional R-factors R are based 
 on F, with F set to zero for negative F^2^. The threshold expression of 
 F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F^2^ are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger.
 
 An AFIX 66 command was used to restrain the geometry of the axle
 aromatic ring to approximate a planar hexagon with C-C bonds of 1.36 A 
 and C-C-C bond angles of 120 deg. Electron density due to atoms of the
 macrocyclic 24C6 ring were diffuse due to the various conformations possible
 and dynamics of the ring which resulted in significant disorder. DFIX and
 DANG commands were used to restrain the C-C, C-O, C-C-C, O-C-C and O-C-C 
 angles in the ring in order to achieve a suitable model. SIMU commands were
 used to distribute the electron density evenly amongst the C and O atoms
 of the macrocyle.
;
_refine_diff_density_max         2.324
_refine_diff_density_min         -0.730
_refine_diff_density_rms         0.215
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   2.363
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     349
_refine_ls_number_reflns         3589
_refine_ls_number_restraints     1575
_refine_ls_restrained_S_all      3.652
_refine_ls_R_factor_all          0.2182
_refine_ls_R_factor_gt           0.1994
_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^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.5549
_refine_ls_wR_factor_ref         0.5617
_reflns_number_gt                2416
_reflns_number_total             3589
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            nchem.1354-s3.cif
_cod_data_source_block           nv219_(SQUEEZE_used_to_remove_H2O_in_void)
_cod_original_sg_symbol_H-M      R-3
_cod_database_code               1508205