Tb-MOF: a naked-eye and regenerable fluorescent probe for selective and quantitative detection of Fe3+and Al3+ions
Zhang, Mengfei; Han, Jing; Wu, Haipeng; Wei, Qing; Xie, Gang; Chen, Sanping; Gao, Shengli; RSC Advances 6 (2016) 94622–; doi:10.1039/C6RA20359K

data_7236256
_publ_section_title
;
 Tb-MOF: a naked-eye and regenerable fluorescent probe for selective and
 quantitative detection of Fe3+and Al3+ions
;
_journal_issue                   97
_journal_name_full               'RSC Advances'
_journal_page_first              94622
_journal_paper_doi               10.1039/C6RA20359K
_journal_volume                  6
_journal_year                    2016
_chemical_formula_moiety         'C44 H32.5 N2.5 O16 Tb3, 3H2 O'
_chemical_formula_sum            'C44 H38.5 N2.5 O19 Tb3'
_chemical_formula_weight         1329.02
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2016-04-18
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2015.08.17 svn.r3210 for OlexSys, GUI svn.r5083)
;
_audit_update_record
;
2016-05-03 deposited with the CCDC.
2016-09-19 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 115.607(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   29.155(3)
_cell_length_b                   11.0593(13)
_cell_length_c                   31.580(5)
_cell_measurement_reflns_used    3203
_cell_measurement_temperature    296.15
_cell_measurement_theta_max      24.27
_cell_measurement_theta_min      2.52
_cell_volume                     9182(2)
_computing_cell_refinement       'SAINT v7.68A (Bruker, 2009)'
_computing_data_reduction        'SAINT v7.68A (Bruker, 2009)'
_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      296.15
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0592
_diffrn_reflns_av_unetI/netI     0.0790
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       36
_diffrn_reflns_limit_h_min       -36
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -39
_diffrn_reflns_number            24948
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.439
_diffrn_reflns_theta_min         1.998
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.643
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.5775
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.0845 before and 0.0534 after correction.
The Ratio of minimum to maximum transmission is 0.7748.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.923
_exptl_crystal_description       block
_exptl_crystal_F_000             5095
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         2.273
_refine_diff_density_min         -0.879
_refine_diff_density_rms         0.180
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.010
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     623
_refine_ls_number_reflns         9386
_refine_ls_number_restraints     42
_refine_ls_restrained_S_all      1.055
_refine_ls_R_factor_all          0.0760
_refine_ls_R_factor_gt           0.0422
_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^)+(0.0441P)^2^+0.9047P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0960
_refine_ls_wR_factor_ref         0.1097
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6275
_reflns_number_total             9386
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6ra20359k2.cif
_cod_data_source_block           Tb_MOFs
_cod_original_formula_sum        'C44 H38.50 N2.50 O19 Tb3'
_cod_database_code               7236256
_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 O(H) groups, All O(H,H) groups
2. Restrained distances
 C30-N3
 1.3 with sigma of 0.02
 N3-C33
 1.3 with sigma of 0.02
 C32-N3
 1.3 with sigma of 0.02
 C30-O10
 1.2 with sigma of 0.02
 H10B-O10
 0.82 with sigma of 0.02
 H10A-O10
 0.82 with sigma of 0.02
 H14-O14 = H15-O15 = H9-O9
 0.82 with sigma of 0.02
 H9-O10_$1
 2.1 with sigma of 0.02
3. Rigid bond restraints
 N3, C30, C31, C32, C33
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
4. Uiso/Uaniso restraints and constraints
Uanis(C33) \\sim Ueq, Uanis(C30) \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.005
Uanis(C32) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(C31) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
5. Others
 Fixed Sof: H10A(0.5) H10B(0.5) N3(0.5) C30(0.5) C31(0.5) H31A(0.5) H31B(0.5)
 H31C(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)
6.a Riding coordinates:
 O9(H9)
6.b Rotating group:
 O10(H10A,H10B)
6.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C6(H6), C7(H7), C9(H9A), C10(H10), C15(H15A), C16(H16),
 C19(H19), C20(H20), C23(H23), C24(H24), C26(H26), C27(H27), C34(H34), C35(H35),
  C36(H36), C37(H37), C38(H38), C39(H39), C41(H41), C42(H42), C45(H45), C46(H46)
6.d Idealised Me refined as rotating group:
 C31(H31A,H31B,H31C), C32(H32A,H32B,H32C), C33(H33A,H33B,H33C)
;
_shelx_fab_checksum              88451
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'