Efficient and selective removal of Pb2+ from aqueous solution by using a O− functionalized metal-organic framework
Jiang, Wen; Yu, Cai-Xia; Yu, Ming-Xuan; Ding, Jing; Song, Jian-Guo; Sun, Xueqin; Liu, Lei-Lei; Dalton Transactions  (2022) –; doi:10.1039/D2DT01117D

data_7710436
_publ_section_title
;
 Efficient and selective removal of Pb2+ from aqueous solution by using a
 O&#x2212; functionalized metal-organic framework
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D2DT01117D
_journal_year                    2022
_chemical_formula_moiety         'C25 H21 N4 O8.5 Pr'
_chemical_formula_sum            'C25 H21 N4 O8.5 Pr'
_chemical_formula_weight         654.37
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2022-04-28
_audit_creation_method
;
Olex2 1.5-dev
(compiled 2022.04.21 svn.rca3783a0 for OlexSys, GUI svn.r6444)
;
_audit_update_record
;
2022-05-08 deposited with the CCDC.	2022-06-07 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 93.15(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.455(3)
_cell_length_b                   8.7878(18)
_cell_length_c                   20.761(4)
_cell_measurement_reflns_used    7738
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      25.56
_cell_measurement_theta_min      2.52
_cell_volume                     2997.6(10)
_computing_cell_refinement       'Bruker SAINT (Bruker, 2003)'
_computing_data_collection       'Bruker APEX2 (Bruker, 2005)'
_computing_data_reduction        'Bruker SAINT (Bruker, 2003)'
_computing_molecular_graphics    'Olex2 1.5-dev (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-dev (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS-2013 (Sheldrick, 2008)'
_diffrn_ambient_temperature      296.15
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0532
_diffrn_reflns_av_unetI/netI     0.0388
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            29334
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        24.999
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_min         2.517
_exptl_absorpt_coefficient_mu    1.675
_exptl_absorpt_correction_T_max  0.846
_exptl_absorpt_correction_T_min  0.785
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.450
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rod
_exptl_crystal_F_000             1304
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.694
_refine_diff_density_min         -1.186
_refine_diff_density_rms         0.083
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     581
_refine_ls_number_reflns         5276
_refine_ls_number_restraints     607
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0433
_refine_ls_R_factor_gt           0.0317
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0389P)^2^+1.0983P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0716
_refine_ls_wR_factor_ref         0.0749
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4234
_reflns_number_total             5276
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt01117d2.cif
_cod_data_source_block           t
_cod_original_cell_volume        2997.7(11)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_original_formula_sum        'C25 H21 N4 O8.50 Pr'
_cod_database_code               7710436
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.850
_shelx_estimated_absorpt_t_min   0.787
_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, All C(H,H,H,H,H,H) groups
2. Restrained distances
 C8-C9 \\sim C8A-C9A
 with sigma of 0.02
 C4-N1 \\sim N1-C6
 with sigma of 0.001
 C17-C19 \\sim C17A-C19A
 with sigma of 0.04
 C8-O4 \\sim C8A-O4A
 with sigma of 0.02
 C15-C17 \\sim C15A-C17A
 with sigma of 0.04
 C8-O5 \\sim C8A-O5A
 with sigma of 0.02
 C9-C10 \\sim C9A-C10A
 with sigma of 0.02
 C9-C14 \\sim C9A-C14A
 with sigma of 0.02
 C19-C21 \\sim C19A-C21A
 with sigma of 0.04
 C10-C11 \\sim C10A-C11A
 with sigma of 0.02
 C12-C14 \\sim C12A-C14A
 with sigma of 0.04
 C11-C12 \\sim C11A-C12A
 with sigma of 0.02
 C12-C13 \\sim C12A-C13A
 with sigma of 0.02
 C16-N3 \\sim C16A-N3A
 with sigma of 0.04
 C12-N2 \\sim C12A-N2A
 with sigma of 0.02
 C18-C20 \\sim C18A-C20A
 with sigma of 0.04
 C11-N2 \\sim C11A-N2A
 with sigma of 0.04
 C13-C14 \\sim C13A-C14A
 with sigma of 0.02
 C15-C16 \\sim C15A-C16A
 with sigma of 0.02
 C15-C20 \\sim C15A-C20A
 with sigma of 0.02
 C15-N3 \\sim C15A-N3A
 with sigma of 0.02
 C16-C18 \\sim C16A-C18A
 with sigma of 0.04
 C16-C17 \\sim C16A-C17A
 with sigma of 0.02
 C18-O8 \\sim C18A-O8A
 with sigma of 0.04
 C17-C18 \\sim C17A-C18A
 with sigma of 0.02
 C20-N3 \\sim C20A-N3A
 with sigma of 0.04
 C18-C19 \\sim C18A-C19A
 with sigma of 0.02
 C18-C21 \\sim C18A-C21A
 with sigma of 0.02
 O4-O5 \\sim O4A-O5A
 with sigma of 0.04
 C19-C20 \\sim C19A-C20A
 with sigma of 0.02
 C21-O7 \\sim C21A-O7A
 with sigma of 0.02
 C21-O8 \\sim C21A-O8A
 with sigma of 0.02
 N2-N3 \\sim N2A-N3A
 with sigma of 0.02
 C12-N3 \\sim C12A-N3A
 with sigma of 0.04
 C13-N2 \\sim C13A-N2A
 with sigma of 0.04
 C15-C19 \\sim C15A-C19A
 with sigma of 0.04
 C15-N2 \\sim C15A-N2A
 with sigma of 0.04
 C16-C20 \\sim C16A-C20A
 with sigma of 0.04
 C8-C10 \\sim C8A-C10A
 with sigma of 0.04
 C17-C21 \\sim C17A-C21A
 with sigma of 0.04
 C8-C14 \\sim C8A-C14A
 with sigma of 0.04
 C18-O7 \\sim C18A-O7A
 with sigma of 0.04
 C9-C11 \\sim C9A-C11A
 with sigma of 0.04
 C9-C13 \\sim C9A-C13A
 with sigma of 0.04
 C9-O4 \\sim C9A-O4A
 with sigma of 0.04
 C9-O5 \\sim C9A-O5A
 with sigma of 0.04
 C10-C12 \\sim C10A-C12A
 with sigma of 0.04
 C10-C14 \\sim C10A-C14A
 with sigma of 0.04
 O7-O8 \\sim O7A-O8A
 with sigma of 0.04
 C11-C13 \\sim C11A-C13A
 with sigma of 0.04
 C22-N4 \\sim C22A-N4A
 with sigma of 0.02
 N4-O9 \\sim N4A-O9A
 with sigma of 0.04
 Pr1-O9 \\sim Pr1-O9A
 with sigma of 0.02
 C24-N4 \\sim C24A-N4A
 with sigma of 0.02
 C25-N4 \\sim C25-N4A
 with sigma of 0.02
 Pr1-C22 \\sim Pr1-C22A
 with sigma of 0.04
 C24-C25 \\sim C24A-C25
 with sigma of 0.04
 C22-C24 \\sim C22A-C24A
 with sigma of 0.04
 C22-C25 \\sim C22A-C25
 with sigma of 0.04
 C23-N4 \\sim C23A-N4A
 with sigma of 0.04
 C23-O9 \\sim C23A-O9A
 with sigma of 0.04
 C22-C23 \\sim C22A-C23A
 with sigma of 0.02
 C22-O9 \\sim C22A-O9A
 with sigma of 0.02
3. Restrained planarity
 N1, N1_$1, O3, O3_$1
 with sigma of 0.001
4. Uiso/Uaniso restraints and constraints
Uanis(O3) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C3) \\sim Ueq, Uanis(C4) \\sim Ueq, Uanis(C5) \\sim Ueq, Uanis(C6) \\sim
Ueq, Uanis(O3) \\sim Ueq, Uanis(N1) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(O10) \\sim Ueq, Uanis(O6) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(O8A) \\sim Ueq, Uanis(O7) \\sim Ueq: with sigma of 0.001 and sigma for
terminal atoms of 0.002
Uanis(O1) \\sim Ueq, Uanis(O2) \\sim Ueq, Uanis(O2) \\sim Ueq, Uanis(O1) \\sim
Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C8) \\sim Ueq, Uanis(C9A) \\sim Ueq, Uanis(C9) \\sim Ueq, Uanis(C8A)
\\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(C18) \\sim Ueq, Uanis(C21) \\sim Ueq: with sigma of 0.001 and sigma for
terminal atoms of 0.002
Uanis(C17A) \\sim Ueq, Uanis(C18A) \\sim Ueq: with sigma of 0.001 and sigma for
terminal atoms of 0.002
5. Rigid body (RIGU) restrains
 N3, C8, C9, O4, O5, C10, C14, C11, C13, C12, N2, C15, O6, C16, C20, C17, C19,
 C18, C21, O7, O8
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C1, C2, O1, O2, C3, C7, C4, C6, C5, N1, O3
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O10, C15A, N3A, C16A, C20A, N2A, C17A, C19A, C12A, C18A, C11A, C13A, C21A,
 C10A, C14A, O7A, O8A, C9A, C8A, O4A, O5A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C22, C23, N4, O9, C24, C25, N4A, C22A, C24A, C23A, O9A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Sof(C15A)=Sof(C8A)=Sof(C9A)=Sof(O4A)=Sof(O5A)=Sof(C10A)=Sof(H10A)=Sof(C14A)=
 Sof(H14A)=Sof(C11A)=Sof(H11A)=Sof(C13A)=Sof(H13A)=Sof(C12A)=Sof(N2A)=Sof(N3A)=
 Sof(C16A)=Sof(H16A)=Sof(C20A)=Sof(H20A)=Sof(C17A)=Sof(H17A)=Sof(C19A)=
 Sof(H19A)=Sof(C18A)=Sof(C21A)=Sof(O7A)=Sof(O8A)=Sof(O10)=1-FVAR(1)
 Sof(C8)=Sof(C9)=Sof(C10)=Sof(H10)=Sof(C11)=Sof(H11)=Sof(C12)=Sof(C13)=
 Sof(H13)=Sof(C14)=Sof(H14)=Sof(C15)=Sof(C16)=Sof(H16)=Sof(C17)=Sof(H17)=
 Sof(C18)=Sof(C19)=Sof(H19)=Sof(C20)=Sof(H20)=Sof(C21)=Sof(N2)=Sof(N3)=Sof(O4)=
 Sof(O5)=Sof(O6)=Sof(O7)=Sof(O8)=FVAR(1)
 Sof(H25D)=Sof(H25E)=Sof(H25F)=Sof(C22A)=Sof(C23A)=Sof(H23D)=Sof(H23E)=
 Sof(H23F)=Sof(C24A)=Sof(H24D)=Sof(H24E)=Sof(H24F)=Sof(N4A)=Sof(O9A)=1-FVAR(2)
 Sof(C22)=Sof(C23)=Sof(H23A)=Sof(H23B)=Sof(H23C)=Sof(C24)=Sof(H24A)=Sof(H24B)=
 Sof(H24C)=Sof(H25A)=Sof(H25B)=Sof(H25C)=Sof(N4)=Sof(O9)=FVAR(2)
 Fixed Sof: O3(0.5)
7.a Aromatic/amide H refined with riding coordinates:
 C4(H4), C3(H3), C7(H7), C6(H6), C10(H10), C11(H11), C13(H13), C14(H14),
 C16(H16), C17(H17), C19(H19), C20(H20), C10A(H10A), C14A(H14A), C11A(H11A),
 C13A(H13A), C16A(H16A), C20A(H20A), C17A(H17A), C19A(H19A)
7.b Fitted hexagon refined as free rotating group:
 C5(C4,C3,C2,C7,C6)
7.c Idealised Me refined as rotating group:
 C23(H23A,H23B,H23C), C24(H24A,H24B,H24C), C25(H25A,H25B,H25C), C25(H25D,H25E,
 H25F), C23A(H23D,H23E,H23F), C24A(H24D,H24E,H24F)
;
_shelx_res_checksum              5454
_shelx_hkl_checksum              78202
_olex2_submission_special_instructions 'No special instructions were received'