Incorporation of an A1/A2-Difunctionalized Pillar[5]arene into a Metal-Organic Framework
Nathan L. Strutt; David Fairen-Jimenez; Julien Iehl; Marianne B. Lalonde; Randall Q. Snurr; Omar K. Farha; Joseph T. Hupp; J. Fraser Stoddart; Journal of the American Chemical Society 134 (2012) 17436–17439; doi:10.1021/ja3082523

data_4118825
_publ_section_title
;
 Incorporation of an A1/A2-Difunctionalized Pillar[5]arene into a
 Metal-Organic Framework
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              17436
_journal_page_last               17439
_journal_paper_doi               10.1021/ja3082523
_journal_volume                  134
_journal_year                    2012
_chemical_formula_sum            'C60 H61 N O13'
_chemical_formula_weight         1004.10
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2012-08-06 # Formatted by publCIF
;
_cell_angle_alpha                90.00
_cell_angle_beta                 97.2640(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.5211(2)
_cell_length_b                   34.3107(4)
_cell_length_c                   11.87650(10)
_cell_measurement_reflns_used    9663
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      134.313
_cell_measurement_theta_min      6.655
_cell_volume                     5869.73(12)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.977
_diffrn_measured_fraction_theta_max 0.977
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.1128
_diffrn_reflns_av_sigmaI/netI    0.0621
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       40
_diffrn_reflns_limit_k_min       -40
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            39135
_diffrn_reflns_theta_full        67.54
_diffrn_reflns_theta_max         67.54
_diffrn_reflns_theta_min         2.58
_exptl_absorpt_coefficient_mu    0.651
_exptl_absorpt_correction_T_max  0.9534
_exptl_absorpt_correction_T_min  0.7670
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, Bruker'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.136
_exptl_crystal_description       columnar
_exptl_crystal_F_000             2128
_exptl_crystal_size_max          0.43
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.07
_platon_squeeze_details
;
Diffuse, disordered solvent molecules could not be adequately modeled.  The
bypass procedure in Platon (Spek, 1990) was used to remove the electronic
contribution from these solvents. The total potential solvent accessible void 
volume was 516 Ang^3^ and the electron count / cell = 117. As the exact solvent
content is not known, the reported formula reflects only the atoms used in the 
refinement.
;
_refine_diff_density_max         0.666
_refine_diff_density_min         -0.457
_refine_diff_density_rms         0.076
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.979
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     679
_refine_ls_number_reflns         10348
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.979
_refine_ls_R_factor_all          0.0669
_refine_ls_R_factor_gt           0.0574
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1120P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1587
_refine_ls_wR_factor_ref         0.1648
_reflns_number_gt                8108
_reflns_number_total             10348
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja3082523_si_003.cif
_cod_data_source_block           n1469a_0m
_cod_database_code               4118825