A molecular shuttle that operates inside a metal-organic framework
Kelong Zhu; Christopher A. O'Keefe; V. Nicholas Vukotic; Robert W. Schurko; Stephen J. Loeb; Nature Chemistry 7 (2015) 514–519; doi:10.1038/nchem.2258

data_1520106
_publ_section_title
;
 A molecular shuttle that operates inside a metal-organic framework
;
_journal_name_full               'Nature Chemistry'
_journal_page_first              514
_journal_page_last               519
_journal_paper_doi               10.1038/nchem.2258
_journal_volume                  7
_journal_year                    2015
_chemical_formula_moiety         'C192 H177 N12 O50 Zn8''B3 F12''C32 H96 O16'
_chemical_formula_sum            'C224 H273 B3 F12 N12 O66 Zn8'
_chemical_formula_weight         4972.92
_space_group_crystal_system      trigonal
_space_group_IT_number           155
_space_group_name_Hall           'R 3 2"'
_space_group_name_H-M_alt        'R 3 2 :H'
_symmetry_space_group_name_Hall  'R 3 2"'
_symmetry_space_group_name_H-M   'R 3 2 :H'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            3
_cell_length_a                   33.030(4)
_cell_length_b                   33.030(4)
_cell_length_c                   28.099(4)
_cell_measurement_reflns_used    235
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      23.257
_cell_measurement_theta_min      2.136
_cell_volume                     26548(6)
_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-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.794
_diffrn_measured_fraction_theta_max 0.998
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0846
_diffrn_reflns_av_unetI/netI     0.0515
_diffrn_reflns_laue_measured_fraction_full 0.794
_diffrn_reflns_laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       36
_diffrn_reflns_limit_h_min       -36
_diffrn_reflns_limit_k_max       36
_diffrn_reflns_limit_k_min       -36
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
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_diffrn_reflns_point_group_measured_fraction_full 0.792
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         23.257
_diffrn_reflns_theta_min         2.136
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.595
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6245
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            pale_yellow
_exptl_crystal_density_diffrn    0.933
_exptl_crystal_description       block
_exptl_crystal_F_000             7776
_exptl_crystal_size_max          0.260
_exptl_crystal_size_mid          0.180
_exptl_crystal_size_min          0.080
_platon_squeeze_details
;
 The unit cell was calculated to contain 3 BF4 anions
 which could not be located and an estimated 48 molecules
 of ethanol. These were treated as a diffuse 
 contribution to the overall scattering without specific
 atom positions by SQUEEZE/PLATON
;
_refine_diff_density_max         0.567
_refine_diff_density_min         -0.308
_refine_diff_density_rms         0.075
_refine_ls_abs_structure_details
;
 Flack x determined using 1988 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   0.079(11)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.997
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     466
_refine_ls_number_reflns         8490
_refine_ls_number_restraints     223
_refine_ls_restrained_S_all      0.998
_refine_ls_R_factor_all          0.1311
_refine_ls_R_factor_gt           0.0782
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.2000P)^2^]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2135
_refine_ls_wR_factor_ref         0.2814
_reflns_Friedel_coverage         0.887
_reflns_friedel_fraction_full    0.790
_reflns_friedel_fraction_max     0.999
_reflns_number_gt                5182
_reflns_number_total             8490
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            nchem.2258-s3.cif
_cod_data_source_block           UWDM4_BF4
_cod_original_cell_volume        26549(7)
_cod_database_code               1520106
_shelx_estimated_absorpt_t_min   0.861
_shelx_estimated_absorpt_t_max   0.954
_shelxl_version_number           2013-2
_shelx_res_checksum              1499
_shelx_hkl_checksum              35972
_shelx_fab_checksum              73943