Development of Metal-Organic Nanotubes Exhibiting Low-Temperature, Reversible Exchange of Confined "Ice Channels"
Daniel K. Unruh; Kyle Gojdas; Anna Libo; Tori Z. Forbes; Journal of the American Chemical Society 135 (2013) 7398–7401; doi:10.1021/ja400303f

data_4119759
_publ_contact_author_address
;Department of Chemistry
University of Iowa
Chemistry Building W374
Iowa City, IA 52242
;
_publ_contact_author_email       tori-forbes@uiowa.edu
_publ_contact_author_fax         319-335-1270
_publ_contact_author_name        'Tori Z. Forbes'
_publ_contact_author_phone       319-384-1320
_publ_section_title
;
 Development of Metal-Organic Nanotubes Exhibiting Low-Temperature,
 Reversible Exchange of Confined "Ice Channels"
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              7398
_journal_page_last               7401
_journal_paper_doi               10.1021/ja400303f
_journal_volume                  135
_journal_year                    2013
_chemical_formula_sum            'C60 H102 N18 O72 U6'
_chemical_formula_weight         3655.78
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           147
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  '-P 3'
_symmetry_space_group_name_H-M   'P -3'
_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            1
_cell_length_a                   22.5338(10)
_cell_length_b                   22.5338(10)
_cell_length_c                   6.5999(4)
_cell_measurement_reflns_used    9698
_cell_measurement_temperature    210(2)
_cell_measurement_theta_max      28.59
_cell_measurement_theta_min      2.76
_cell_volume                     2902.3(3)
_computing_cell_refinement       'APEX2 (Bruker AXS, 2006)'
_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_data_reduction        'APEX2 (Bruker AXS, 2006)'
_computing_molecular_graphics    'CrystalMaker v2.5.0'
_computing_publication_material  'PLATON (Spek, 2009)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      210(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'CCD 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  0.0314
_diffrn_reflns_av_sigmaI/netI    0.0141
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            55033
_diffrn_reflns_theta_full        28.64
_diffrn_reflns_theta_max         28.64
_diffrn_reflns_theta_min         2.76
_exptl_absorpt_coefficient_mu    8.450
_exptl_absorpt_correction_T_max  0.466
_exptl_absorpt_correction_T_min  0.253
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.099
_exptl_crystal_description       blocky
_exptl_crystal_F_000             1716
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.14
_refine_diff_density_max         1.176
_refine_diff_density_min         -0.650
_refine_diff_density_rms         0.122
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.091
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     234
_refine_ls_number_reflns         4951
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.091
_refine_ls_R_factor_all          0.0201
_refine_ls_R_factor_gt           0.0183
_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^)+(0.0320P)^2^+4.3918P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0540
_refine_ls_wR_factor_ref         0.0547
_reflns_number_gt                4712
_reflns_number_total             4951
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja400303f_si_006.cif
_cod_data_source_block           hexanes
_cod_database_code               4119759