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_7209004
_publ_section_title
;
 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            'C70 H48 O21 Zn4'
_chemical_formula_weight         1486.64
_chemical_name_common            12C4
_chemical_name_systematic
;
?
;
_space_group_IT_number           138
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  '-P 4ac 2ac'
_symmetry_space_group_name_H-M   'P 42/n c m :2'
_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            4
_cell_length_a                   21.4901(11)
_cell_length_b                   21.4901(11)
_cell_length_c                   42.883(4)
_cell_measurement_reflns_used    1526
_cell_measurement_temperature    143(2)
_cell_measurement_theta_max      21.23
_cell_measurement_theta_min      1.96
_cell_volume                     19804(2)
_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      143(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  0.1495
_diffrn_reflns_av_sigmaI/netI    0.0833
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       46
_diffrn_reflns_limit_l_min       -39
_diffrn_reflns_number            77217
_diffrn_reflns_theta_full        22.60
_diffrn_reflns_theta_max         22.60
_diffrn_reflns_theta_min         1.90
_exptl_absorpt_coefficient_mu    0.504
_exptl_absorpt_correction_T_max  0.7525
_exptl_absorpt_correction_T_min  0.7525
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    0.499
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       cube
_exptl_crystal_F_000             3024
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.60
_exptl_crystal_size_min          0.60
_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 2485 electron counts in
voids in each unit cell, 328 electrons are from 4
unresolved crown ethers, and 2157 electrons from
estimated solvents (about 34 DMF in one unit cell,
8.5 DMF per [Zn4O(C26H22O8)3]).

;
_refine_diff_density_max         0.598
_refine_diff_density_min         -0.657
_refine_diff_density_rms         0.072
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.945
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     255
_refine_ls_number_reflns         6856
_refine_ls_number_restraints     47
_refine_ls_restrained_S_all      0.970
_refine_ls_R_factor_all          0.1245
_refine_ls_R_factor_gt           0.0767
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1327P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2138
_refine_ls_wR_factor_ref         0.2301
_reflns_number_gt                3309
_reflns_number_total             6856
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2ce26401c.txt
_cod_data_source_block           mof-bc4
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Tetragonal' changed to 'tetragonal'
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 
;
_cod_original_cell_volume        19805(2)
_cod_original_sg_symbol_H-M      P42/ncm
_cod_database_code               7209004