An unprecedented dynamic porous metal-organic framework assembled from fivefold interlocked closed nanotubes with selective gas adsorption behaviors
Ping Ju; Long Jiang; Tong-Bu Lu; Chemical communications (Cambridge, England) 49 (2013) 1820–1822; doi:10.1039/c3cc38519a

data_7108883
_publ_section_title
;
 An unprecedented dynamic porous metal-organic framework assembled from
 fivefold interlocked closed nanotubes with selective gas adsorption
 behaviors
;
_journal_issue                   18
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              1820
_journal_page_last               1822
_journal_paper_doi               10.1039/c3cc38519a
_journal_volume                  49
_journal_year                    2013
_chemical_formula_sum            'C87 H153 N17 Ni3 O27'
_chemical_formula_weight         2045.39
_chemical_name_systematic
;
?
;
_space_group_IT_number           120
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  'I -4 -2c'
_symmetry_space_group_name_H-M   'I -4 c 2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2012-11-24
_audit_creation_method
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CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET)
(compiled Aug 3 2011,13:03:54)
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_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   30.233(2)
_cell_length_b                   30.233(2)
_cell_length_c                   22.671(3)
_cell_measurement_reflns_used    2364
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      64.6608
_cell_measurement_theta_min      2.9208
_cell_volume                     20722(3)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET)
(compiled Aug 3 2011,13:03:54)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET)
(compiled Aug 3 2011,13:03:54)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET)
(compiled Aug 3 2011,13:03:54)
;
_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      150(2)
_diffrn_detector_area_resol_mean 10.5058
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_source         'Enhance Ultra (Cu) X-ray Source'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_R_equivalents  0.0559
_diffrn_reflns_av_sigmaI/netI    0.0441
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            15419
_diffrn_reflns_theta_full        63.00
_diffrn_reflns_theta_max         63.00
_diffrn_reflns_theta_min         3.81
_exptl_absorpt_coefficient_mu    1.288
_exptl_absorpt_correction_T_max  0.6760
_exptl_absorpt_correction_T_min  0.6139
_exptl_absorpt_correction_type   multi-scan
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CrysAlisPro, Agilent Technologies,
Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET)
(compiled Aug 3 2011,13:03:54)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            pink
_exptl_crystal_density_diffrn    1.311
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             8752
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.36
_exptl_crystal_size_min          0.33
_platon_squeeze_details
;
The diffraction of 1 was very weak due to the presence of
highly disordered pendent arm of azamacrocyclic ligand
and lattice water molecules,
and the attempt to locate the highly disordered pendent arms
and water molecules was unsuccessful.
Therefore, the SQUEEZE routine of PLATON was applied to
remove the diffraction contributed from the disordered section
(twelve disordered water molecules
and one and a half disordered 2-aminobutan-1-ol groups
of azamacrocyclic ligand per asymmetric unit).
The final formula was calculated from the TGA combined
with elemental analysis data.
;
_refine_diff_density_max         0.507
_refine_diff_density_min         -0.439
_refine_diff_density_rms         0.052
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.40(11)
_refine_ls_extinction_coef       0.0000069(8)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.077
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     847
_refine_ls_number_reflns         7405
_refine_ls_number_restraints     116
_refine_ls_restrained_S_all      1.074
_refine_ls_R_factor_all          0.1800
_refine_ls_R_factor_gt           0.1244
_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^)+(0.0058P)^2^+71.4156P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1931
_refine_ls_wR_factor_ref         0.2066
_reflns_number_gt                2827
_reflns_number_total             7405
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3cc38519a.txt
_cod_data_source_block           1
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Tetragonal' changed to 'tetragonal'
according to
/usr/data/users/saulius/automatic-downloads/retrospective/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 
;
_cod_original_cell_volume        20722(4)
_cod_original_sg_symbol_H-M      I-4c2
_cod_database_code               7108883