A thermostable terbium(iii) complex with high fluorescence quantum yields
Chen, Bao-Li; Sun, Yan-Mei; Xiang, Hua; Lin, Mu-Xiong; Li, Jian-Han; Huang, Yong-Liang; New Journal of Chemistry 46 (2022) 11021–11024; doi:10.1039/D2NJ01250B

data_7061556
_publ_section_title
;
 A thermostable terbium(iii) complex with high fluorescence quantum yields
;
_journal_issue                   23
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              11021
_journal_page_last               11024
_journal_paper_doi               10.1039/D2NJ01250B
_journal_volume                  46
_journal_year                    2022
_chemical_formula_moiety         '3(C6 H16 N), C21 H16 N6 O27 Tb2'
_chemical_formula_sum            'C39 H64 N9 O27 Tb2'
_chemical_formula_weight         1408.83
_space_group_crystal_system      monoclinic
_space_group_IT_number           5
_space_group_name_Hall           'C 2y'
_space_group_name_H-M_alt        'C 1 2 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_audit_creation_date             2022-04-05
_audit_creation_method
;
Olex2 1.5-dev
(compiled 2022.03.10 svn.r54f81f84 for OlexSys, GUI svn.r6444)
;
_audit_update_record
;
2022-05-08 deposited with the CCDC.	2022-05-10 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 120.5930(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   19.3502(3)
_cell_length_b                   11.14440(10)
_cell_length_c                   14.4386(2)
_cell_measurement_reflns_used    4093
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      73.758
_cell_measurement_theta_min      3.556
_cell_volume                     2680.23(7)
_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 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    'olex2.solve 1.5-dev (Bourhis et al., 2015)'
_diffrn_ambient_temperature      150.15
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       'Omega scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0251
_diffrn_reflns_av_unetI/netI     0.0278
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.983
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            8333
_diffrn_reflns_point_group_measured_fraction_full 0.785
_diffrn_reflns_point_group_measured_fraction_max 0.756
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         73.758
_diffrn_reflns_theta_min         3.556
_exptl_absorpt_coefficient_mu    13.634
_exptl_absorpt_correction_T_max  0.6852
_exptl_absorpt_correction_T_min  0.3426
_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_colour            colorless
_exptl_crystal_density_diffrn    1.746
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1414
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.801
_refine_diff_density_min         -0.903
_refine_diff_density_rms         0.075
_refine_ls_abs_structure_details
;
 Flack x determined using 1242 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.011(4)
_refine_ls_extinction_coef       0.00044(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     441
_refine_ls_number_reflns         4093
_refine_ls_number_restraints     198
_refine_ls_restrained_S_all      1.061
_refine_ls_R_factor_all          0.0254
_refine_ls_R_factor_gt           0.0251
_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^)+(0.0453P)^2^+2.6677P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0669
_refine_ls_wR_factor_ref         0.0673
_reflns_Friedel_coverage         0.460
_reflns_Friedel_fraction_full    0.546
_reflns_Friedel_fraction_max     0.504
_reflns_number_gt                4028
_reflns_number_total             4093
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2nj01250b2.cif
_cod_data_source_block           6
_cod_depositor_comments          'Adding full bibliography for 7061556.cif.'
_cod_database_code               7061556
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.685
_shelx_estimated_absorpt_t_min   0.343
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2. Restrained distances
 N5-C41
 1.5 with sigma of 0.005
 N5-C39
 1.5 with sigma of 0.005
 N5-C14 = N5-C41 = N5-C39
 1.5 with sigma of 0.01
 N5-C13
 2.533 with sigma of 0.01
 C42-N5 = N5-C40
 2.533 with sigma of 0.01
 N4-C37
 1.5 with sigma of 0.005
 N4-C33
 1.5 with sigma of 0.005
 N4-C31
 1.5 with sigma of 0.005
 C37-C38A
 1.53 with sigma of 0.001
 C31-C32
 1.53 with sigma of 0.005
 C33-C34
 1.53 with sigma of 0.005
 C39-C40
 1.53 with sigma of 0.005
 C41-C42
 1.53 with sigma of 0.005
 C41-C39
 2.55 with sigma of 0.005
 C38A-N4
 2.533 with sigma of 0.01
 C14-C41
 2.533 with sigma of 0.01
 C14-C39 = C39-C41
 2.533 with sigma of 0.01
 C42-C41 = C13-C14 = C40-C39
 1.52 with sigma of 0.01
 N5-C42 \\sim N5-C40
 with sigma of 0.005
 N4-C37 \\sim N4A-C37A
 with sigma of 0.02
 N4-C33 \\sim N4A-C33A
 with sigma of 0.02
 C34-C33 \\sim C34A-C33A
 with sigma of 0.02
 C33-C31 \\sim C33A-C31A
 with sigma of 0.04
 C33-C37 \\sim C33A-C37A
 with sigma of 0.04
 C31-C37 \\sim C31A-C37A
 with sigma of 0.04
 N4-C31 \\sim N4A-C31A
 with sigma of 0.02
 C38A-C37 \\sim C38B-C37A
 with sigma of 0.02
 C34-N4 \\sim C34A-N4A
 with sigma of 0.04
 N4-C32 \\sim N4A-C32A
 with sigma of 0.04
 N4-C38A \\sim N4A-C38B
 with sigma of 0.04
 C32-C31 \\sim C32A-C31A
 with sigma of 0.02
3. Restrained planarity
 C10, C9, C11, C12
 with sigma of 0.005
4. Rigid bond restraints
 C10, O7
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.005
 C33, C34
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.005
 C31, C32
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.005
 C37
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.005
 N4, C37
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.005
5. Uiso/Uaniso restraints and constraints
C10 \\sim O7: within 2A with sigma of 0.02 and sigma for terminal atoms of 0.01
within 2A
C33 \\sim C34: within 2A with sigma of 0.02 and sigma for terminal atoms of
0.01 within 2A
C31 \\sim C32: within 2A with sigma of 0.02 and sigma for terminal atoms of
0.01 within 2A
C38B \\sim C38A: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02 within 2A
Uanis(C39) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(C37) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(C42) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(C10) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(C39) = Uanis(N5)
Uanis(C42) = Uanis(C41)
Uanis(C10) = Uanis(O7)
6. Rigid body (RIGU) restrains
 C14, C40, C39, N5, C41, C42, C13
 with sigma for 1-2 distances of 0.0005 and sigma for 1-3 distances of 0.0005
 C38A, C34, C33, N4, C37, C31, C32
 with sigma for 1-2 distances of 0.0005 and sigma for 1-3 distances of 0.0005
 N4A, C33A, C31A, C37A, C34A, C32A, C38B
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C38A, C34, C33, N4, C31, C37, C32
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
7. Others
 Sof(N4A)=Sof(H4AA)=Sof(C34A)=Sof(H34D)=Sof(H34E)=Sof(H34F)=Sof(C33A)=
 Sof(H33C)=Sof(H33D)=Sof(C31A)=Sof(H31C)=Sof(H31D)=Sof(C37A)=Sof(H37C)=
 Sof(H37D)=Sof(C32A)=Sof(H32D)=Sof(H32E)=Sof(H32F)=Sof(C38B)=Sof(H38D)=
 Sof(H38E)=Sof(H38F)=1-FVAR(1)
 Sof(C34)=Sof(H34A)=Sof(H34B)=Sof(H34C)=Sof(N4)=Sof(H4A)=Sof(C32)=Sof(H32A)=
 Sof(H32B)=Sof(H32C)=Sof(C33)=Sof(H33A)=Sof(H33B)=Sof(C31)=Sof(H31A)=Sof(H31B)=
 Sof(C38A)=Sof(H38A)=Sof(H38B)=Sof(H38C)=Sof(C37)=Sof(H37A)=Sof(H37B)=FVAR(1)
 Fixed Sof: C40(0.5) H40A(0.5) H40B(0.5) H40C(0.5) N5(0.5) H5(0.5) C41(0.5)
 H41A(0.5) H41B(0.5) C42(0.5) H42A(0.5) H42B(0.5) H42C(0.5) C39(0.5) H39A(0.5)
 H39B(0.5) O7(0.5) H10(0.5) C13(0.5) H13A(0.5) H13B(0.5) H13C(0.5) C14(0.5)
 H14A(0.5) H14B(0.5)
8.a Riding coordinates:
 O7(H7), C10(H10), C13(H13A,H13B,H13C)
8.b Ternary CH refined with riding coordinates:
 N5(H5), N4(H4A), N4A(H4AA)
8.c Secondary CH2 refined with riding coordinates:
 C41(H41A,H41B), C33(H33A,H33B), C31(H31A,H31B), C39(H39A,H39B), C37(H37A,
 H37B), C14(H14A,H14B), C33A(H33C,H33D), C31A(H31C,H31D), C37A(H37C,H37D)
8.d Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C15(H15), C6(H6), C11(H11), C12(H12)
8.e Idealised Me refined as rotating group:
 C40(H40A,H40B,H40C), C42(H42A,H42B,H42C), C34(H34A,H34B,H34C), C32(H32A,H32B,
 H32C), C38A(H38A,H38B,H38C), C34A(H34D,H34E,H34F), C32A(H32D,H32E,H32F),
 C38B(H38D,H38E,H38F)
8.f Idealised tetrahedral OH refined as rotating group:
 O14(H14)
;
_shelx_res_checksum              73231
_olex2_submission_special_instructions 'No special instructions were received'