Distinct interpenetrated metal‒organic frameworks constructed from crown ether-based strut analogue
Liu, Lei; Wang, Xiaojun; Zhang, Quan; Li, Qiaowei; Zhao, Yanli; CrystEngComm 15 (2013) 841–; doi:10.1039/c2ce26401c

data_7209005
_publ_section_title
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 Distinct interpenetrated metal--organic frameworks constructed from crown
 ether-based strut analogue
;
_journal_issue                   5
_journal_name_full               CrystEngComm
_journal_page_first              841
_journal_paper_doi               10.1039/c2ce26401c
_journal_volume                  15
_journal_year                    2013
_chemical_formula_sum            'C60 H24 O13 Zn4'
_chemical_formula_weight         1214.27
_chemical_name_common            15C5
_chemical_name_systematic
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?
;
_space_group_IT_number           229
_symmetry_cell_setting           cubic
_symmetry_space_group_name_Hall  '-I 4 2 3'
_symmetry_space_group_name_H-M   'I m -3 m'
_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                90.00
_cell_formula_units_Z            2
_cell_length_a                   21.4744(13)
_cell_length_b                   21.4744(13)
_cell_length_c                   21.4744(13)
_cell_measurement_reflns_used    362
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      23.08
_cell_measurement_theta_min      2.21
_cell_volume                     9902.9(10)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_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      153(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       '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  0.1062
_diffrn_reflns_av_sigmaI/netI    0.0338
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            25086
_diffrn_reflns_theta_full        25.16
_diffrn_reflns_theta_max         25.16
_diffrn_reflns_theta_min         1.90
_exptl_absorpt_coefficient_mu    0.496
_exptl_absorpt_correction_T_max  0.8860
_exptl_absorpt_correction_T_min  0.8654
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    0.407
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       cube
_exptl_crystal_F_000             1216
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.25
_platon_squeeze_details
;
Very little remaining electron density was left, because
of the highly disordered nature of the crown ethers and
solvent molecules. The highly diffused electron density
makes impossible to locate these atoms. SQUEEZE shows
about 1852 electron counts in voids in each unit cell,
636 electrons are from 6 unresolved crown ethers, and
1216 electrons from estimated solvents (about 19 DMF in
one unit cell, 9.5 DMF per [Zn4O(C28H26O9)3] )).
;
_refine_diff_density_max         0.365
_refine_diff_density_min         -0.409
_refine_diff_density_rms         0.053
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.105
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     44
_refine_ls_number_reflns         907
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.129
_refine_ls_R_factor_all          0.1460
_refine_ls_R_factor_gt           0.0921
_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^)+(0.1989P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2759
_refine_ls_wR_factor_ref         0.3150
_reflns_number_gt                550
_reflns_number_total             907
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2ce26401c.txt
_cod_data_source_block           mof-bc5
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Cubic' changed to 'cubic' according
to /home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary
named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 
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_cod_original_sg_symbol_H-M      Im-3m
_cod_database_code               7209005