A sixfold interpenetrated microporous MOF constructed from heterometallic tetranuclear cluster exhibiting selective gas adsorption.
Li, Yun-Wu; Wang, Li-Fu; He, Kun-Huan; Chen, Qiang; Bu, Xian-He; Dalton transactions (Cambridge, England : 2003) 40 (2011) 10319–10321; doi:10.1039/c1dt10554j

data_7016649
_publ_section_title
;
 A sixfold interpenetrated microporous MOF constructed from
 heterometallic tetranuclear cluster exhibiting selective gas
 adsorption.
;
_journal_issue                   40
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              10319
_journal_page_last               10321
_journal_paper_doi               10.1039/c1dt10554j
_journal_volume                  40
_journal_year                    2011
_chemical_formula_sum            'C135 H111 Cd6 N24 Na2 O30'
_chemical_formula_weight         3269.86
_chemical_name_systematic
;
?
;
_space_group_IT_number           182
_symmetry_cell_setting           hexagonal
_symmetry_space_group_name_Hall  'P 6c 2c'
_symmetry_space_group_name_H-M   'P 63 2 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                120.00
_cell_formula_units_Z            2
_cell_length_a                   18.643(3)
_cell_length_b                   18.643(3)
_cell_length_c                   24.945(5)
_cell_measurement_temperature    123(2)
_cell_volume                     7508(2)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      123(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       \w
_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  0.0677
_diffrn_reflns_av_sigmaI/netI    0.0295
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            69805
_diffrn_reflns_theta_full        27.11
_diffrn_reflns_theta_max         27.11
_diffrn_reflns_theta_min         2.06
_exptl_absorpt_coefficient_mu    0.916
_exptl_absorpt_correction_T_max  0.8380
_exptl_absorpt_correction_T_min  0.8102
_exptl_absorpt_correction_type   'multi-scan(SADABS; Sheldrick,1996)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.446
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3278
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.20
_platon_squeeze_details
;

In order to subtract the contribution from the disordered solvent molecules,
the SQUEEZE command was applied, which gave a new HKL file.
The number of located electrons, 152 in four voids per unit cell,
is included in the formula, formula weight, calculated density, and F(000).
These residual electron density were assigned to five dimethylammonium ions.
So SQUEEZE removed five dimethylammonium ions per unit cell.
This value calculated based upon charge balance considerations,
volume/count_electrons analysis, combining with elemental analyses,
and TG analyses. (One dimethylammonium ion would give 26 e).
There are two formula units in one cell, so one formula unit contains 2.5
disordered dimethylammonium ions, which combining with the 1.5 determined
dimethylammonium ions, giving to 4 dimethylammonium ions per formula unit.
Considering charge balance, these 4 dimethylammonium ions were assigned to three
dimethylammonium cations and one dimethylammonium anion.
So the tentative formula
for this compound is presented as in the text.
See refs. (a) O. V. Dolomanov, D. B. Cordes, N. R. Champness, A. J. Blake,
L. R. Hanton, G. B. Jameson, M. Schroder and C. Wilson. Chem. Commun.,
2004, 642; (b) Y. Du, A. L. Thompson and D. O. Hare.Chem. Commun. 2008, 5987;
(c) Y. F. Bi, X. T. Wang, W. P. Liao, X. F. Wang, X. W. Wang, H. J. Zhang,
and S. Gao, J. Am. Chem. Soc. 2009, 131, 11650.

PLAT306_ALERT_2_A Isolated Oxygen Atom (H-atoms Missing ?) .... O1W
PLAT430_ALERT_2_A Short Inter D...A Contact O1W .. O5 .. 2.26 Ang
PLAT430_ALERT_2_A Short Inter D...A Contact O1W .. O3 .. 2.39 Ang
PLAT430_ALERT_2_A Short Inter D...A Contact O1W .. O3 .. 2.39 Ang
PLAT430_ALERT_2_B Short Inter D...A Contact O1W .. O2 .. 2.80 Ang
PLAT430_ALERT_2_B Short Inter D...A Contact O1W .. O2 .. 2.80 Ang
These alerts arise because of missing water molecules in the model resulting
in apparent large structural voids and missing H-bonds
;
_refine_diff_density_max         0.758
_refine_diff_density_min         -0.842
_refine_diff_density_rms         0.121
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.02(5)
_refine_ls_extinction_coef       0.0027(3)
_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   1.108
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     322
_refine_ls_number_reflns         5533
_refine_ls_number_restraints     154
_refine_ls_restrained_S_all      1.131
_refine_ls_R_factor_all          0.0648
_refine_ls_R_factor_gt           0.0593
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0872P)^2^+6.3601P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1537
_refine_ls_wR_factor_ref         0.1581
_reflns_number_gt                5059
_reflns_number_total             5533
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c1dt10554j.txt
_cod_data_source_block           x
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Hexagonal' changed to 'hexagonal'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_sg_symbol_H-M      P6322
_cod_database_code               7016649