An excellent colorimetric and “turn off” fluorescent probe for tetrahydrofuran based on a luminescent macrocyclic samarium(iii) complex
Yang, Zhuo-Ran; Feng, Cheng-Cheng; Nie, Peng-Peng; Chen, Ting-Ting; Zhang, Lin-Feng; Ma, Shuang; Shen, Yin-Jing; Lu, Ze-Ying; Lin, Meng-Lu; Zhang, Kun; The Analyst  (2019) –; doi:10.1039/C9AN01037H

data_1552136
_publ_section_title
;
 An excellent colorimetric and &#x201C;turn off&#x201D; fluorescent probe
 for tetrahydrofuran based on a luminescent macrocyclic samarium(iii)
 complex
;
_journal_name_full               'The Analyst'
_journal_paper_doi               10.1039/C9AN01037H
_journal_year                    2019
_chemical_formula_moiety         'C30 H31 Cl2 F N5 O10 Sm'
_chemical_formula_sum            'C30 H31 Cl2 F N5 O10 Sm'
_chemical_formula_weight         861.85
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2018-04-22
_audit_creation_method
;
Olex2 1.2
(compiled 2018.04.18 svn.r3501 for OlexSys, GUI svn.r5488)
;
_audit_update_record
;
2019-03-14 deposited with the CCDC.    2019-07-25 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 96.846(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.1220(12)
_cell_length_b                   13.6316(11)
_cell_length_c                   20.7727(17)
_cell_measurement_reflns_used    7677
_cell_measurement_temperature    291(2)
_cell_measurement_theta_max      26.39
_cell_measurement_theta_min      2.45
_cell_volume                     3689.2(5)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_diffrn_ambient_temperature      291.0
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0945
_diffrn_reflns_av_unetI/netI     0.0648
_diffrn_reflns_Laue_measured_fraction_full 0.987
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            42718
_diffrn_reflns_point_group_measured_fraction_full 0.987
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.467
_diffrn_reflns_theta_min         2.162
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.799
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6714
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0839 before and 0.0669 after correction.
The Ratio of minimum to maximum transmission is 0.9007.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'yellow green'
_exptl_crystal_density_diffrn    1.552
_exptl_crystal_description       block
_exptl_crystal_F_000             1724
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.14
_refine_diff_density_max         1.203
_refine_diff_density_min         -2.090
_refine_diff_density_rms         0.202
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     413
_refine_ls_number_reflns         7511
_refine_ls_number_restraints     42
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.1066
_refine_ls_R_factor_gt           0.0760
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0900P)^2^+43.0850P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1834
_refine_ls_wR_factor_ref         0.1993
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5424
_reflns_number_total             7511
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9an01037h2.cif
_cod_data_source_block           Sm-2e
_cod_database_code               1552136
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.787
_shelx_estimated_absorpt_t_min   0.652
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups, All N(H) groups
2. Restrained distances
 C4-C7 \\sim C7-F1B
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C4) \\sim Ueq, Uanis(F1B) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(F1A) \\sim Ueq, Uanis(C7) \\sim Ueq, Uanis(C6) \\sim Ueq, Uanis(C3) \\sim
Ueq, Uanis(C2) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of
0.02
Uanis(C4) = Uanis(F1B)
Uanis(C4) = Uanis(C3) = Uanis(C1) = Uanis(C5) = Uanis(C2) = Uanis(C6) =
Uanis(F1A) = Uanis(F1B) = Uanis(C0AA) = Uanis(C1AA) = Uanis(C6AA) = Uanis(C5AA)
= Uanis(C4AA) = Uanis(C3AA) = Uanis(C2AA) = Uanis(C7)
4. Others
 Sof(H8BC)=Sof(H8BD)=Sof(F1B)=Sof(C0AA)=Sof(H0AA)=Sof(H0AB)=Sof(C1AA)=
 Sof(C6AA)=Sof(H6AA)=Sof(C5AA)=Sof(H5AA)=Sof(C4AA)=Sof(C3AA)=Sof(H3AA)=
 Sof(C2AA)=Sof(H2AA)=1-FVAR(1)
 Sof(C4)=Sof(C3)=Sof(H3)=Sof(C1)=Sof(C7)=Sof(H7A)=Sof(H7B)=Sof(H8AA)=Sof(H8AB)=
 Sof(C5)=Sof(H5)=Sof(C2)=Sof(H2)=Sof(C6)=Sof(H6)=Sof(F1A)=FVAR(1)
5.a Ternary CH refined with riding coordinates:
 N1(H1)
5.b Secondary CH2 refined with riding coordinates:
 C18(H18A,H18B), C22(H22A,H22B), C30(H30A,H30B), C21(H21A,H21B), C19(H19A,
 H19B), C17(H17A,H17B), C20(H20A,H20B), C7(H7A,H7B), C9(H9A,H9B), C8(H8AA,H8AB),
  C8(H8BC,H8BD), C0AA(H0AA,H0AB)
5.c Aromatic/amide H refined with riding coordinates:
 C25(H25), C3(H3), C23(H23), C16(H16), C27(H27), C13(H13), C5(H5), C2(H2),
 C11(H11), C6(H6), C6AA(H6AA), C5AA(H5AA), C3AA(H3AA), C2AA(H2AA)
5.d Fitted hexagon refined as free rotating group:
 C1AA(C6AA,C5AA,C4AA,C3AA,C2AA)
;
_shelx_res_checksum              5074
_shelx_fab_checksum              10768
_olex2_submission_special_instructions 'No special instructions were received'