pH-stable Eu- and Tb-organic-frameworks mediated by ionic liquid for aqueous-phase detection of 2,4,6-trinitrophenol (TNP)
Qin, Jian-Hua; Wang, Huarui; Han, Min-Le; chang, Xin-Hong; ma, lufang; Dalton Trans.  (2017) –; doi:10.1039/C7DT03433D

data_7044469
_publ_section_title
;
 pH-stable Eu- and Tb-organic-frameworks mediated by ionic liquid for
 aqueous-phase detection of 2,4,6-trinitrophenol (TNP)
;
_journal_name_full               'Dalton Trans.'
_journal_paper_doi               10.1039/C7DT03433D
_journal_year                    2017
_chemical_formula_moiety         '0.5(C118 H72 N12 O26 Tb4), H2 O'
_chemical_formula_sum            'C59 H38 N6 O14 Tb2'
_chemical_formula_weight         1372.79
_chemical_name_systematic
;
 ?
;
_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   mixed
_atom_sites_solution_primary     dual
_audit_block_doi                 10.5517/ccdc.csd.cc1ptgcb
_audit_creation_date             2017-09-29
_audit_creation_method
;
Olex2 1.2-alpha
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2017-09-30 deposited with the CCDC.
2017-10-13 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 110.015(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   8.0636(8)
_cell_length_b                   16.5777(17)
_cell_length_c                   20.0148(19)
_cell_measurement_reflns_used    9896
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      28.24
_cell_measurement_theta_min      2.49
_cell_volume                     2513.9(4)
_computing_cell_refinement       'SAINT v7.34A (Bruker, 200?)'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'SAINT v7.34A (Bruker, 200?)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      296.15
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.980
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0303
_diffrn_reflns_av_unetI/netI     0.0335
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.980
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            20084
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.980
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.499
_diffrn_reflns_theta_min         2.490
_diffrn_standards_decay_%        none
_diffrn_standards_interval_count none
_diffrn_standards_interval_time  none
_diffrn_standards_number         none
_exptl_absorpt_coefficient_mu    2.870
_exptl_absorpt_correction_T_max  0.5259
_exptl_absorpt_correction_T_min  0.4332
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.814
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1352
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.24
_refine_diff_density_max         2.614
_refine_diff_density_min         -1.721
_refine_diff_density_rms         0.159
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.194
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     367
_refine_ls_number_reflns         5677
_refine_ls_number_restraints     39
_refine_ls_restrained_S_all      1.211
_refine_ls_R_factor_all          0.0515
_refine_ls_R_factor_gt           0.0433
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0002P)^2^+19.7523P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0910
_refine_ls_wR_factor_ref         0.0938
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4890
_reflns_number_total             5677
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt03433d2.cif
_cod_data_source_block           Tb
_cod_database_code               7044469
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.546
_shelx_estimated_absorpt_t_min   0.433
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, H7 of O7
 At 1.5 times of:
  H8 of O8
2. Rigid bond restraints
 N2, C23, C24
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
3. Uiso/Uaniso restraints and constraints
N2 \\sim C23 \\sim C24: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.02
Uanis(O8) \\sim Ueq, Uanis(N2) \\sim Ueq, Uanis(C23) \\sim Ueq, Uanis(C24)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
4.a Riding coordinates:
 O7(H7), O8(H8)
4.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C7(H7A), C10(H10), C11(H11), C13(H13), C14(H14), C16(H16),
 C18(H18), C21(H21), C22(H22), C23(H23), C24(H24), C25(H25), C26(H26), C28(H28),
  C29(H29), C30(H30)
;
_shelx_res_checksum              57496
_olex2_submission_special_instructions 'No special instructions were received'