Triple-Wavelength-Region Luminescence Sensing Based on a Color-Tunable Emitting Lanthanide Metal Organic Framework.
Wang, Xin-Yu; Yao, Xu; Huang, Qiang; Li, Yu-Xin; An, Guang-Hui; Li, Guang-Ming; Analytical chemistry 90 (2018) 6675–6682; doi:10.1021/acs.analchem.8b00494

data_1552961
_publ_section_title
;
 Triple-Wavelength-Region Luminescence Sensing Based on a Color-Tunable
 Emitting Lanthanide Metal Organic Framework.
;
_journal_issue                   11
_journal_name_full               'Analytical chemistry'
_journal_page_first              6675
_journal_page_last               6682
_journal_paper_doi               10.1021/acs.analchem.8b00494
_journal_volume                  90
_journal_year                    2018
_chemical_formula_moiety         'C22 H23 N2 O9 Tb'
_chemical_formula_sum            'C22 H23 N2 O9 Tb'
_chemical_formula_weight         618.35
_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   geom
_audit_creation_date             2018-01-19
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_cell_angle_alpha                90.000(5)
_cell_angle_beta                 97.284(5)
_cell_angle_gamma                90.000(5)
_cell_formula_units_Z            8
_cell_length_a                   28.614(5)
_cell_length_b                   14.383(5)
_cell_length_c                   13.644(5)
_cell_measurement_reflns_used    9362
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      29.6239
_cell_measurement_theta_min      3.2014
_cell_volume                     5570(3)
_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_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  MoK\a
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0510
_diffrn_reflns_av_unetI/netI     0.0362
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            19514
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        24.998
_diffrn_reflns_theta_max         24.998
_diffrn_reflns_theta_min         3.208
_exptl_absorpt_coefficient_mu    2.585
_exptl_absorpt_correction_T_max  0.596
_exptl_absorpt_correction_T_min  0.529
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.475
_exptl_crystal_description       block
_exptl_crystal_F_000             2448
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.055
_refine_diff_density_min         -1.502
_refine_diff_density_rms         0.095
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     311
_refine_ls_number_reflns         4901
_refine_ls_number_restraints     160
_refine_ls_restrained_S_all      1.090
_refine_ls_R_factor_all          0.0330
_refine_ls_R_factor_gt           0.0275
_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^)+(0.0311P)^2^+22.9034P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0693
_refine_ls_wR_factor_ref         0.0743
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4319
_reflns_number_total             4901
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            3-tb_sq.cif
_cod_data_source_block           3-tb_sq
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               1552961
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.626
_shelx_estimated_absorpt_t_min   0.564
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C18-N1
 1.45 with sigma of 0.02
 C17-N1
 1.45 with sigma of 0.02
 N1-C16
 1.369 with sigma of 0.02
 C20-N2
 1.45 with sigma of 0.02
 C21-N2
 1.45 with sigma of 0.02
 C18-C16
 2.442 with sigma of 0.04
 C17-C16
 2.442 with sigma of 0.04
 C18-C17
 2.511 with sigma of 0.04
 N2-C19
 1.369 with sigma of 0.04
 C20-C19
 2.442 with sigma of 0.04
 C19-C21
 2.442 with sigma of 0.04
 C21-C20
 2.551 with sigma of 0.04
3. Rigid bond restraints
 C16, C17, C18, N1, O9
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C19, C20, C21, N2, O8
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
C16 \\sim C17 \\sim C18 \\sim N1 \\sim O9: within 3.8A with sigma of 0.04 and
sigma for terminal atoms of 0.08
C19 \\sim C20 \\sim C21 \\sim N2 \\sim O8: within 3.8A with sigma of 0.04 and
sigma for terminal atoms of 0.08
Uanis(C21) \\sim Ueq, Uanis(C18) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
5.a Secondary CH2 refined with riding coordinates:
 C8(H8A,H8B)
5.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C7(H7), C10(H10), C11(H11), C13(H13), C14(H14), C16(H16),
 C19(H19)
5.c Idealised Me refined as rotating group:
 C17(H17A,H17B,H17C), C18(H18A,H18B,H18C), C20(H20A,H20B,H20C), C21(H21A,H21B,
 H21C)
;
_shelx_res_checksum              25289
_shelx_hkl_checksum              6808
_shelx_fab_checksum              70815
_olex2_submission_special_instructions 'No special instructions were received'