Two microporous Co<sup>II</sup>-MOFs with dual active sites for highly selective adsorption of CO<sub>2</sub>/CH<sub>4</sub> and CO<sub>2</sub>/N<sub>2</sub>.
Ma, Hui-Yan; Zhang, Yong-Zheng; Yan, Hui; Zhang, Wen-Jie; Li, Yun-Wu; Wang, Su-Na; Li, Da-Cheng; Dou, Jian-Min; Li, Jian-Rong; Dalton transactions (Cambridge, England : 2003) 48 (2019) 13541–13545; doi:10.1039/c9dt02694k

data_7700921
_publ_section_title
;
 Two microporous Co<sup>II</sup>-MOFs with dual active sites for highly
 selective adsorption of CO<sub>2</sub>/CH<sub>4</sub> and
 CO<sub>2</sub>/N<sub>2</sub>.
;
_journal_issue                   36
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              13541
_journal_page_last               13545
_journal_paper_doi               10.1039/c9dt02694k
_journal_volume                  48
_journal_year                    2019
_chemical_formula_sum            'C36 H68 Co N6 O17'
_chemical_formula_weight         915.89
_space_group_crystal_system      monoclinic
_space_group_IT_number           13
_space_group_name_Hall           '-P 2yc'
_space_group_name_H-M_alt        'P 1 2/c 1'
_symmetry_space_group_name_Hall  '-P 2yc'
_symmetry_space_group_name_H-M   'P 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2019-05-25 deposited with the CCDC.    2019-08-23 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 95.69(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.601(4)
_cell_length_b                   9.3797(19)
_cell_length_c                   18.630(4)
_cell_measurement_reflns_used    26897
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      24.996
_cell_measurement_theta_min      3.090
_cell_volume                     3408.3(12)
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       \w
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.2573
_diffrn_reflns_av_unetI/netI     0.2056
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            26897
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        24.996
_diffrn_reflns_theta_max         24.996
_diffrn_reflns_theta_min         3.090
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.552
_exptl_absorpt_correction_T_max  0.926
_exptl_absorpt_correction_T_min  0.905
_exptl_absorpt_correction_type   'multi-scan(SADABS; Sheldrick,1996)'
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.113
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1144
_exptl_crystal_size_max          0.180
_exptl_crystal_size_mid          0.160
_exptl_crystal_size_min          0.140
_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, 174 in two voids per unit cell,
is included in the formula, formula weight, calculated density, and F(000).
These residual electron density were assigned to three DMAC and three water.
So SQUEEZE removed three DMAC and three water per unit cell.
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.

PLAT430_ALERT_2_A Short Inter D...A Contact  O1W .. O2 .. 2.28 Ang  
PLAT430_ALERT_2_A Short Inter D...A Contact  O1W .. O8 .. 2.30 Ang  
PLAT430_ALERT_2_A Short Inter D...A Contact  O1W .. O4 .. 2.40 Ang  
PLAT430_ALERT_2_A Short Inter D...A Contact  O2W .. O9 .. 2.14 Ang  
PLAT430_ALERT_2_A Short Inter D...A Contact  O2W .. O3 .. 2.29 Ang  
PLAT430_ALERT_2_A Short Inter D...A Contact  O2W .. O6 .. 2.32 Ang  
PLAT430_ALERT_2_A Short Inter D...A Contact  O2W .. O7 .. 2.42 Ang  
These alerts arise because of missing water molecules in the model resulting
in apparent large structural voids and missing H-bonds.

RINTA01_ALERT_3_A  The value of Rint is greater than 0.25  Rint given   0.257
PLAT020_ALERT_3_A The Value of Rint is Greater Than 0.12 ....... 0.257 Report
Due to the limited crystal quality, the more solvents, and the relatively 
high ?\%restraints?+- in the both compounds, which all result the higher R value.
;
_refine_diff_density_max         0.950
_refine_diff_density_min         -0.608
_refine_diff_density_rms         0.145
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.130
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     352
_refine_ls_number_reflns         5995
_refine_ls_number_restraints     116
_refine_ls_restrained_S_all      1.197
_refine_ls_R_factor_all          0.2352
_refine_ls_R_factor_gt           0.1492
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3669
_refine_ls_wR_factor_ref         0.4167
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2730
_reflns_number_total             5995
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt02694k2.cif
_cod_data_source_block           LCU-105
_cod_depositor_comments
'Adding full bibliography for 7700921--7700922.cif.'
_cod_database_code               7700921
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.907
_shelx_estimated_absorpt_t_max   0.927
_shelx_res_checksum              20535
_shelx_fab_checksum              25864