Template-directed synthesis of a luminescent Tb-MOF material for highly selective Fe3+ and Al3+ ion detection and VOC vapor sensing
Chen, Di-Ming; Zhang, Nan-Nan; Liu, Chun-Sen; Du, Miao; Journal of Materials Chemistry C 5 (2017) 2311–; doi:10.1039/C6TC05349A

data_7236459
_publ_section_title
;
 Template-directed synthesis of a luminescent Tb-MOF material for highly
 selective Fe3+ and Al3+ ion detection and VOC vapor sensing
;
_journal_issue                   9
_journal_name_full               'Journal of Materials Chemistry C'
_journal_page_first              2311
_journal_paper_doi               10.1039/C6TC05349A
_journal_volume                  5
_journal_year                    2017
_chemical_formula_moiety         '0.17(C168 H96 O60 Tb6), C2 H4 N4, C2 H8 N'
_chemical_formula_sum            'C32 H28 N5 O10 Tb'
_chemical_formula_weight         801.51
_space_group_crystal_system      hexagonal
_space_group_IT_number           181
_space_group_name_Hall           'P 64 2 (0 0 2)'
_space_group_name_H-M_alt        'P 64 2 2'
_atom_sites_solution_hydrogens   mixed
_audit_block_doi                 10.5517/ccdc.csd.cc1n2f49
_audit_creation_date             2016-12-08
_audit_creation_method
;
Olex2 1.2
(compiled 2016.11.30 svn.r3356 for OlexSys, GUI svn.r5269)
;
_audit_update_record
;
2016-12-09 deposited with the CCDC.
2017-01-30 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            6
_cell_length_a                   15.1834(4)
_cell_length_b                   15.1834(4)
_cell_length_c                   26.5282(9)
_cell_measurement_reflns_used    6786
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.8680
_cell_measurement_theta_min      4.0760
_cell_volume                     5296.3(3)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_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(2)
_diffrn_detector_area_resol_mean 16.2542
_diffrn_measured_fraction_theta_full 0.9955
_diffrn_measured_fraction_theta_max 0.9973
_diffrn_measurement_details
;
  1 omega  -31.00   75.00   1.0000   45.7300
omega____ theta____ kappa____ phi______ frames
    -       18.4204    0.0000  -30.0000 106

  2 omega  -23.00    2.00   1.0000   45.7300
omega____ theta____ kappa____ phi______ frames
    -      -18.4985  -77.0000  -90.0000 25

  3 omega  -79.00  -44.00   1.0000   45.7300
omega____ theta____ kappa____ phi______ frames
    -      -18.4985  -77.0000  -90.0000 35
;
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0442181000
_diffrn_orient_matrix_UB_12      -0.0479749000
_diffrn_orient_matrix_UB_13      0.0038274000
_diffrn_orient_matrix_UB_21      -0.0226406000
_diffrn_orient_matrix_UB_22      0.0080044000
_diffrn_orient_matrix_UB_23      -0.0216063000
_diffrn_orient_matrix_UB_31      0.0209549000
_diffrn_orient_matrix_UB_32      -0.0232918000
_diffrn_orient_matrix_UB_33      -0.0152947000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0275
_diffrn_reflns_av_unetI/netI     0.0205
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            14753
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.009
_diffrn_reflns_theta_max         25.009
_diffrn_reflns_theta_min         3.098
_diffrn_source                   'Enhance (Mo) X-ray Source'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.063
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.91783
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_density_diffrn    1.508
_exptl_crystal_F_000             2400
_refine_diff_density_max         1.030
_refine_diff_density_min         -0.622
_refine_diff_density_rms         0.104
_refine_ls_abs_structure_details
;
 Flack x determined using 1004 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.003(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.124
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     242
_refine_ls_number_reflns         3121
_refine_ls_number_restraints     46
_refine_ls_restrained_S_all      1.138
_refine_ls_R_factor_all          0.0456
_refine_ls_R_factor_gt           0.0381
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0507P)^2^+21.9300P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1045
_refine_ls_wR_factor_ref         0.1120
_reflns_Friedel_coverage         0.653
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                2770
_reflns_number_total             3121
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6tc05349a2.cif
_cod_data_source_block           1
_cod_original_sg_symbol_Hall     'P 64 2c (0 0 -1)'
_cod_database_code               7236459
_chemical_oxdiff_formula         'C H O N Tb'
_reflns_odcompleteness_completeness 99.55
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups, All N(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 H1B_$1-H19
 2.1 with sigma of 0.02
 N10-O
 2.9 with sigma of 0.001
 C3-N4
 1.47 with sigma of 0.01
 C3-C1
 2.28 with sigma of 0.01
 N4-C3 = N4-C1
 1.41 with sigma of 0.01
 N10-N10_$2
 2.1 with sigma of 0.01
 N2-N10 = N10-C0AA = N10-C1AA
 1.39 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
C1 \\sim N4 \\sim C3: within 2A with sigma of 0.005 and sigma for terminal
atoms of 0.01
Uanis(C1) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C1) \\sim Ueq, Uanis(C3) \\sim Ueq: with sigma of 0.001 and sigma for
terminal atoms of 0.002
Uanis(C0AA) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(C3) \\sim Ueq, Uanis(N4) \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.01
4. Others
 Fixed Sof: H6A(0.5) H6B(0.5) N2(0.5) H2(0.5) C0AA(0.5) H0AA(0.5) C3(0.5)
 H3A(0.5) H3B(0.5) H3C(0.5) N4(0.5) H4A(0.5) H4B(0.5) C1(0.5) H1A(0.5) H1B(0.5)
 H1C(0.5)
5.a Riding coordinates:
 N4(H4A,H4B)
5.b Ternary CH refined with riding coordinates:
 N2(H2), C0AA(H0AA)
5.c Me refined with riding coordinates:
 C3(H3A,H3B,H3C)
5.d Aromatic/amide H refined with riding coordinates:
 C18(H18), C19(H19), C22(H22), C23(H23), C30(H30), C31(H31), C(H), C2AA(H2AA)
5.e X=CH2 refined with riding coordinates:
 N6(H6A,H6B)
5.f Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C)
;
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'