A self-made portable separation device based on 2-D MOF nanosheets for the efficient separation of dyes in solutions
Li, Anqi; Ma, Xiaofan; Ma, Jie; Yuan, Qingyi; Zhang, Jun; Xuan, Xiaopeng; CrystEngComm 23 (2021) 3989–3994; doi:10.1039/D1CE00251A

data_7242694
_publ_section_title
;
 A self-made portable separation device based on 2-D MOF nanosheets for
 the efficient separation of dyes in solutions
;
_journal_issue                   22
_journal_name_full               CrystEngComm
_journal_page_first              3989
_journal_page_last               3994
_journal_paper_doi               10.1039/D1CE00251A
_journal_volume                  23
_journal_year                    2021
_chemical_formula_moiety         'C28 H24 Cu2 N2 O10'
_chemical_formula_sum            'C28 H24 Cu2 N2 O10'
_chemical_formula_weight         675.59
_space_group_crystal_system      orthorhombic
_space_group_IT_number           52
_space_group_name_Hall           '-P 2a 2bc'
_space_group_name_H-M_alt        'P n n a'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2019-06-26
_audit_creation_method
;
Olex2 1.2-alpha
(compiled 2018.07.26 svn.r3523 for OlexSys, GUI svn.r5532)
;
_audit_update_record
;
2020-10-06 deposited with the CCDC.	2021-04-21 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   24.2206(10)
_cell_length_b                   18.2735(10)
_cell_length_c                   17.7634(8)
_cell_measurement_reflns_used    2878
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      73.1700
_cell_measurement_theta_min      3.4390
_cell_volume                     7862.0(6)
_computing_cell_refinement       'CrysAlisPro 1.171.39.32a (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.32a (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.32a (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_temperature      293.15
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_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   -115.00 -48.00   0.50   15.00    --  -43.55 -57.00 -30.00  134
  2  \w   -120.00 -77.00   0.50   35.00    --  -90.25 -77.00 -60.00   86
  3  \w    -70.00  -8.00   0.50   15.00    --  -43.55  77.00-120.00  124
  4  \w     27.00  67.00   0.50   15.00    --   43.55 -57.00 -60.00   80
  5  \w     46.00 137.00   0.50   35.00    --  111.75 -79.00  65.95  182
  6  \w     81.00 111.00   0.50   35.00    --  111.75 -80.00 124.64   60
  7  \w     47.00  75.00   0.50   35.00    --  111.75 -80.00 124.64   56
  8  \w    -23.00   2.00   0.50   15.00    --   43.55 -57.00 -60.00   50
  9  \w     89.00 166.00   0.50   35.00    --  111.75  61.00 120.00  154
 10  \w     88.00 166.00   0.50   35.00    --  111.75  61.00 -30.00  156
 11  \w     83.00 135.00   0.50   35.00    --  111.75  77.00-180.00  104
;
_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      0.0227543000
_diffrn_orient_matrix_UB_12      -0.0808572000
_diffrn_orient_matrix_UB_13      0.0064374000
_diffrn_orient_matrix_UB_21      -0.0836603000
_diffrn_orient_matrix_UB_22      -0.0221639000
_diffrn_orient_matrix_UB_23      0.0000199000
_diffrn_orient_matrix_UB_31      0.0023162000
_diffrn_orient_matrix_UB_32      -0.0083009000
_diffrn_orient_matrix_UB_33      -0.0633189000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0961
_diffrn_reflns_av_unetI/netI     0.1765
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            22364
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        62.500
_diffrn_reflns_theta_max         62.500
_diffrn_reflns_theta_min         3.085
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.715
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.142
_exptl_crystal_description       block
_exptl_crystal_F_000             2752
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.20
_refine_diff_density_max         1.749
_refine_diff_density_min         -0.590
_refine_diff_density_rms         0.120
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.968
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     488
_refine_ls_number_reflns         6256
_refine_ls_number_restraints     895
_refine_ls_restrained_S_all      0.989
_refine_ls_R_factor_all          0.1148
_refine_ls_R_factor_gt           0.0851
_refine_ls_shift/su_max          0.079
_refine_ls_shift/su_mean         0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0162P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1985
_refine_ls_wR_factor_ref         0.2118
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3248
_reflns_number_total             6256
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1ce00251a2.cif
_cod_data_source_block           exp_2308
_cod_depositor_comments          'Adding full bibliography for 7242694.cif.'
_cod_database_code               7242694
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'c h o  n Ni '
_reflns_odcompleteness_completeness 99.62
_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
 Cu1A-O10A = Cu1-O10 = Cu2-O7 = Cu2A-O7A
 2 with sigma of 0.01
 O10A-C26A = O10-C26 = O7-C13 = O7A-C13A
 1.2 with sigma of 0.01
 N1A-C13A = N1-C13 = N1-C15 = N1A-C15A = N1A-C14A = N1-C14 = N2A-C26A = N2-C26
 = N2A-C27A = N2-C27 = N2-C28 = N2A-C28A
 1.46 with sigma of 0.01
 C27A-C26A
 2.5 with sigma of 0.02
 C26A-C28A
 2.5 with sigma of 0.02
 C28A-C27A
 2.5 with sigma of 0.02
 O10A-N2A
 2.5 with sigma of 0.02
3. Restrained planarity
 O10A, C26A, N2A, C28A, C27A
 with sigma of 0.01
 O10, C26, N2, C28, C27
 with sigma of 0.01
4. Uiso/Uaniso restraints and constraints
C4 \\sim C9 \\sim C10 \\sim C19 \\sim C16 \\sim C17 \\sim C22 \\sim C7 \\sim C6
\\sim C21 \\sim C20 \\sim C24 \\sim C8 \\sim C5 \\sim C25 \\sim C3 \\sim C18:
within 2A with sigma of 0.0051 and sigma for terminal atoms of 0.02
Cu1 \\sim Cu2 \\sim O10 \\sim N1 \\sim N2 \\sim C27 \\sim C26 \\sim C13 \\sim
C15 \\sim Cu1A \\sim Cu2A \\sim O10A \\sim N1A \\sim N2A \\sim C27A \\sim C26A
\\sim C28A \\sim C13A \\sim C15A \\sim O7 \\sim C28 \\sim C14 \\sim O7A \\sim
C14A: within 2A with sigma of 0.0051 and sigma for terminal atoms of 0.02
Uanis(C21) \\sim Ueq, Uanis(C20) \\sim Ueq, Uanis(C9) \\sim Ueq, Uanis(C19)
\\sim Ueq, Uanis(C16) \\sim Ueq, Uanis(C17) \\sim Ueq, Uanis(C6) \\sim Ueq,
Uanis(C2) \\sim Ueq, Uanis(C1) \\sim Ueq, Uanis(C3) \\sim Ueq, Uanis(C18) \\sim
Ueq, Uanis(C4) \\sim Ueq, Uanis(C5) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(O7) \\sim Ueq, Uanis(N1) \\sim Ueq, Uanis(C13) \\sim Ueq, Uanis(C14)
\\sim Ueq, Uanis(C15) \\sim Ueq, Uanis(O7A) \\sim Ueq, Uanis(N1A) \\sim Ueq,
Uanis(C13A) \\sim Ueq, Uanis(C14A) \\sim Ueq, Uanis(C15A) \\sim Ueq, Uanis(Cu1)
\\sim Ueq, Uanis(Cu2) \\sim Ueq, Uanis(O10) \\sim Ueq, Uanis(N2) \\sim Ueq,
Uanis(C27) \\sim Ueq, Uanis(C26) \\sim Ueq, Uanis(Cu1A) \\sim Ueq, Uanis(Cu2A)
\\sim Ueq, Uanis(O10A) \\sim Ueq, Uanis(N2A) \\sim Ueq, Uanis(C27A) \\sim Ueq,
Uanis(C26A) \\sim Ueq, Uanis(C28A) \\sim Ueq, Uanis(C28) \\sim Ueq: with sigma
of 0.01 and sigma for terminal atoms of 0.02
Uanis(C12) \\sim Ueq, Uanis(C16) \\sim Ueq, Uanis(C23) \\sim Ueq: with sigma of
0.005 and sigma for terminal atoms of 0.01
5. Rigid body (RIGU) restrains
 C9, C10, C19, C16, C17, C22, C7, C6, C2, C21, C20, C24, C8, C1, C25, C3, C18,
 C4, C5
 with sigma for 1-2 distances of 0.0051 and sigma for 1-3 distances of 0.01
 Cu1, O10, N1, N2, C27, C13, C15, Cu1A, Cu2A, O10A, N1A, N2A, C27A, C26A, C28A,
  C13A, C15A, Cu2, O7, C26, C28, C14, O7A, C14A
 with sigma for 1-2 distances of 0.0051 and sigma for 1-3 distances of 0.01
6. Others
 Sof(Cu1A)=Sof(Cu2A)=Sof(O7A)=Sof(O10A)=Sof(N1A)=Sof(N2A)=Sof(C27A)=Sof(H27D)=
 Sof(H27E)=Sof(H27F)=Sof(C26A)=Sof(H26A)=Sof(C28A)=Sof(H28D)=Sof(H28E)=
 Sof(H28F)=Sof(C13A)=Sof(H13A)=Sof(C14A)=Sof(H14D)=Sof(H14E)=Sof(H14F)=
 Sof(C15A)=Sof(H15D)=Sof(H15E)=Sof(H15F)=1-FVAR(1)
 Sof(Cu1)=Sof(Cu2)=Sof(O7)=Sof(O10)=Sof(N1)=Sof(N2)=Sof(C27)=Sof(H27A)=
 Sof(H27B)=Sof(H27C)=Sof(C26)=Sof(H26)=Sof(C28)=Sof(H28A)=Sof(H28B)=Sof(H28C)=
 Sof(C13)=Sof(H13)=Sof(C14)=Sof(H14A)=Sof(H14B)=Sof(H14C)=Sof(C15)=Sof(H15A)=
 Sof(H15B)=Sof(H15C)=FVAR(1)
7.a Me refined with riding coordinates:
 C27(H27A,H27B,H27C), C28(H28A,H28B,H28C), C14(H14A,H14B,H14C), C15(H15A,H15B,
 H15C), C27A(H27D,H27E,H27F), C28A(H28D,H28E,H28F), C14A(H14D,H14E,H14F),
 C15A(H15D,H15E,H15F)
7.b Aromatic/amide H refined with riding coordinates:
 C4(H4), C10(H10), C17(H17), C26(H26), C7(H7), C21(H21), C20(H20), C24(H24),
 C8(H8), C5(H5), C25(H25), C13(H13), C26A(H26A), C13A(H13A)
;
_shelx_res_checksum              6570
_shelx_hkl_checksum              759
_shelx_fab_checksum              90528
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
;
_oxdiff_exptl_absorpt_empirical_full_max 1.587
_oxdiff_exptl_absorpt_empirical_full_min 0.694