Construction of a metal‒organic framework by octuple intercatenation of discrete icosahedral coordination cages
Shen, Yu; Zhu, Hai-Bin; Hu, Jun; Zhao, Yue; CrystEngComm 17 (2015) 2080–; doi:10.1039/C4CE02207F

data_7219474
_publ_section_title
;
 Construction of a metal--organic framework by octuple intercatenation of
 discrete icosahedral coordination cages
;
_journal_issue                   10
_journal_name_full               CrystEngComm
_journal_page_first              2080
_journal_paper_doi               10.1039/C4CE02207F
_journal_volume                  17
_journal_year                    2015
_chemical_formula_sum            'C132 H79 N3 O66 Pb13 S24'
_chemical_formula_weight         6225.89
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           228
_symmetry_cell_setting           cubic
_symmetry_space_group_name_Hall  '-F 4ud 2vw 3'
_symmetry_space_group_name_H-M   'F d -3 c :2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2015-02-01 deposited with the CCDC.
2015-02-03 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            16
_cell_length_a                   40.110(5)
_cell_length_b                   40.110(5)
_cell_length_c                   40.110(5)
_cell_measurement_temperature    298(2)
_cell_volume                     64529(14)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w 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  0.0606
_diffrn_reflns_av_sigmaI/netI    0.0275
_diffrn_reflns_limit_h_max       51
_diffrn_reflns_limit_h_min       -51
_diffrn_reflns_limit_k_max       51
_diffrn_reflns_limit_k_min       -51
_diffrn_reflns_limit_l_max       51
_diffrn_reflns_limit_l_min       -45
_diffrn_reflns_number            188415
_diffrn_reflns_theta_full        27.56
_diffrn_reflns_theta_max         27.56
_diffrn_reflns_theta_min         1.44
_exptl_absorpt_coefficient_mu    13.916
_exptl_absorpt_correction_T_max  0.1885
_exptl_absorpt_correction_T_min  0.1581
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.563
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             45920
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.18
_platon_squeeze_details
;
In order to subtract the contribution from the disordered solvent molecules,
the SQUEEZE command was applied.
SQUEEZE removed three disordered DMAc and six H2O per formula unit. This valueis calculated based upon volume/count_electrons analysis.
See ref. Bi, Y. F.; Wang, X. T.; Liao, W. P.; Wang, X. F.; Wang, X. W.;
Zhang, H. J.; Gao, S. J. Am. Chem. Soc. 2009, 131, 11650.

CHEMW03_ALERT_2_B WARNING: The ratio of given/expected molecular weight as
            calculated from the _atom_site* data lies outside
            the range 0.95 <> 1.05
           From the CIF: _cell_formula_units_Z                   16
           From the CIF: _chemical_formula_weight          6225.89
           TEST: Calculate formula weight from _atom_site_*
           atom     mass    num     sum
           C        12.01  120.00 1441.32
           H         1.01   24.00   24.19
           O        16.00   57.00  911.94
           S        32.07   24.00  769.58
           Pb      207.20   13.00 2693.60
           N        14.01    0.00    0.00
           Calculated formula weight             5840.64
RESPONSE: This is caused by the given molecular weight being increased
from the atom count to account for disordered DMAc and H2O omitted by SQUEEZE and the hydrogen atoms of water and hydroxide.
;
_refine_diff_density_max         1.280
_refine_diff_density_min         -1.441
_refine_diff_density_rms         0.217
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.087
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     164
_refine_ls_number_reflns         3124
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.087
_refine_ls_R_factor_all          0.0764
_refine_ls_R_factor_gt           0.0504
_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^)+(0.0800P)^2^+1.5500P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1403
_refine_ls_wR_factor_ref         0.1463
_reflns_number_gt                1966
_reflns_number_total             3124
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4ce02207f2.cif
_cod_data_source_block           sr
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Cubic' changed to 'cubic' according
to
/usr/data/users/saulius/crontab/automatic-downloads/rss-feeds/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 3008 2015-01-20 13:52:24Z robertas 

 Adding full bibliography for 7219474.cif.
;
_cod_original_cell_volume        64528(13)
_cod_original_sg_symbol_Hall     '-F 4cvw 2vw 3'
_cod_original_sg_symbol_H-M      'Fd-3c '
_cod_database_code               7219474