A pillar-layered porous CoII-MOF with dual active sites for selective gas adsorption
Gao, Xiang; Zhang, Shan-Shan; Yan, Hui; Li, Yun-Wu; Liu, Qing-Yun; Wang, Xing-Po; Tung, Chen-Ho; Ma, Hui-Yan; Sun, Di; CrystEngComm 20 (2018) 4905–; doi:10.1039/C8CE01118D

data_7231286
_publ_section_title
;
 A pillar-layered porous CoII-MOF with dual active sites for selective gas
 adsorption
;
_journal_issue                   34
_journal_name_full               CrystEngComm
_journal_page_first              4905
_journal_paper_doi               10.1039/C8CE01118D
_journal_volume                  20
_journal_year                    2018
_chemical_formula_moiety
'0.25(C160 H136 Co12 N32 O56), 5(C3 H7 N O), C3 H4 N O'
_chemical_formula_sum            'C58 H73 Co3 N14 O20'
_chemical_formula_weight         1463.09
_space_group_crystal_system      orthorhombic
_space_group_IT_number           62
_space_group_name_Hall           '-P 2ac 2n'
_space_group_name_H-M_alt        'P n m a'
_symmetry_space_group_name_Hall  '-P 2ac 2n'
_symmetry_space_group_name_H-M   'P n m a'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2017-12-12
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5337)
;
_audit_update_record
;
2018-05-01 deposited with the CCDC.
2018-08-03 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.1925(5)
_cell_length_b                   40.2091(13)
_cell_length_c                   9.5480(3)
_cell_measurement_reflns_used    10173
_cell_measurement_temperature    173.00(10)
_cell_measurement_theta_max      76.9030
_cell_measurement_theta_min      4.3480
_cell_volume                     6984.4(4)
_computing_cell_refinement       'CrysAlisPro 1.171.39.30d (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.30d (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.30d (Rigaku OD, 2017)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      173.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -62.00  17.00   1.00    0.80    --  -48.32  57.00  60.00   79
  2  \w    -58.00  27.00   1.00    0.80    --  -48.32  25.00 -48.00   85
  3  \w     56.00  81.00   1.00    0.80    --   48.32  25.00 -48.00   25
  4  \w    102.00 178.00   1.00    4.00    --  107.75  25.00 -48.00   76
  5  \w    -51.00 -16.00   1.00    4.00    --  -86.25  25.00 -48.00   35
  6  \w    -99.00 -64.00   1.00    4.00    --  -86.25  57.00 120.00   35
  7  \w    -60.00 -14.00   1.00    4.00    --  -86.25  57.00 120.00   46
  8  \w     96.00 177.00   1.00    4.00    --  107.75  19.00  30.00   81
  9  \w     36.00  76.00   1.00    4.00    --  107.75 -99.00 150.00   40
 10  \w     85.00 110.00   1.00    4.00    --  107.75 -99.00 150.00   25
 11  \w     83.00 109.00   1.00    4.00    --  107.75 -25.00 147.00   26
 12  \w     42.00 120.00   1.00    4.00    --  107.75 -57.00-120.00   78
 13  \w     35.00 130.00   1.00    4.00    --  107.75 -77.00  30.00   95
 14  \w    -26.00   4.00   1.00    0.80    --   48.32 -25.00 147.00   30
 15  \w   -121.00 -42.00   1.00    0.80    --  -48.32 -25.00 147.00   79
 16  \w   -158.00-101.00   1.00    4.00    --  -86.25 -25.00 147.00   57
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0179518000
_diffrn_orient_matrix_UB_12      0.0367397000
_diffrn_orient_matrix_UB_13      -0.0305867000
_diffrn_orient_matrix_UB_21      -0.0209416000
_diffrn_orient_matrix_UB_22      -0.0091889000
_diffrn_orient_matrix_UB_23      -0.1514445000
_diffrn_orient_matrix_UB_31      -0.0800808000
_diffrn_orient_matrix_UB_32      -0.0058047000
_diffrn_orient_matrix_UB_33      0.0464733000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0895
_diffrn_reflns_av_unetI/netI     0.0527
_diffrn_reflns_Laue_measured_fraction_full 0.986
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       47
_diffrn_reflns_limit_k_min       -48
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            40236
_diffrn_reflns_point_group_measured_fraction_full 0.986
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         67.071
_diffrn_reflns_theta_min         4.398
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    6.183
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.13752
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.30d (Rigaku Oxford Diffraction, 2017)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear pinkish pink'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   pinkish
_exptl_crystal_colour_primary    pink
_exptl_crystal_density_diffrn    1.391
_exptl_crystal_description       plate
_exptl_crystal_F_000             3040
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.385
_refine_diff_density_min         -1.000
_refine_diff_density_rms         0.109
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     459
_refine_ls_number_reflns         6332
_refine_ls_number_restraints     98
_refine_ls_restrained_S_all      1.067
_refine_ls_R_factor_all          0.0847
_refine_ls_R_factor_gt           0.0684
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1066P)^2^+20.6119P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1865
_refine_ls_wR_factor_ref         0.2033
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5021
_reflns_number_total             6332
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8ce01118d2.cif
_cod_data_source_block           171212a
_cod_depositor_comments          'Adding full bibliography for 7231286.cif.'
_cod_database_code               7231286
_shelxl_version_number           2013-4
_chemical_oxdiff_formula         CoCNO
_shelx_estimated_absorpt_t_max   0.836
_shelx_estimated_absorpt_t_min   0.577
_diffrn_oxdiff_ac3_digest_frames
;
019982b01ad8a8ce4f779a1a88808485ad00892204e
;
_diffrn_oxdiff_ac3_digest_hkl
;
0145011aa47b97392f5bfd347ad3405b1634c4
;
_reflns_odcompleteness_completeness 99.86
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 O11-C31
 1.25 with sigma of 0.01
 N8-C32 \\sim N8-C33 \\sim N8-C31
 with sigma of 0.01
 N8A-C33A \\sim N8A-C32A \\sim N8A-C31A
 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
O11A \\sim N8A \\sim C31A \\sim C32A \\sim C33A: within 1.7A with sigma of
0.004 and sigma for terminal atoms of 0.08
O11 \\sim N8 \\sim C31 \\sim C32 \\sim C33 \\sim O11A \\sim N8A \\sim C31A
\\sim C32A \\sim C33A: within 1.7A with sigma of 0.004 and sigma for terminal
atoms of 0.08
C21 \\sim C20 \\sim N4 \\sim C19 \\sim O7: within 1.7A with sigma of 0.004 and
sigma for terminal atoms of 0.008
O9 \\sim N7 \\sim C28 \\sim C29 \\sim C30: within 1.7A with sigma of 0.004 and
sigma for terminal atoms of 0.08
O10 \\sim N6 \\sim C25 \\sim C26 \\sim C27: within 1.7A with sigma of 0.004 and
sigma for terminal atoms of 0.08
4. Others
 Fixed Sof: N7(0.5) C28(0.5) H7A(0.5) H29A(0.5) H29B(0.5) H29C(0.5) C30(0.5)
 H30A(0.5) H30B(0.5) H30C(0.5) H25B(0.5) H25C(0.5) H26B(0.5) H26C(0.5) O11(0.5)
 N8(0.5) C31(0.5) H31(0.5) C32(0.5) H32A(0.5) H32B(0.5) H32C(0.5) C33(0.5)
 H33A(0.5) H33B(0.5) H33C(0.5) O11A(0.5) N8A(0.5) C31A(0.5) H31A(0.5) C32A(0.5)
 C33A(0.5) H33D(0.5) H33E(0.5) H33F(0.5)
5.a Riding coordinates:
 C28(H7A), C29(H29A,H29B,H29C), C30(H30A,H30B,H30C)
5.b Me refined with riding coordinates:
 C25(H25A,H25B,H25C), C26(H26A,H26B,H26C)
5.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C6(H6), C7(H7), C11(H11), C12(H12), C13(H13), C14(H14),
 C15(H15), C16(H16), C18(H18), C19(H19), C22(H22), C27(H27), C31(H31),
 C31A(H31A)
5.d Idealised Me refined as rotating group:
 C20(H20A,H20B,H20C), C21(H21A,H21B,H21C), C23(H23A,H23B,H23C), C24(H24A,H24B,
 H24C), C32(H32A,H32B,H32C), C33(H33A,H33B,H33C), C33A(H33D,H33E,H33F)
;
_shelx_res_checksum              75107
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.863
_oxdiff_exptl_absorpt_empirical_full_min 0.436