Regulation of the Metal Center and Coordinating Anion of Mononuclear Ln(III) Complexes to Promote an Efficient Luminescence Response to Various Organic Solvents
Wang, Hui-Feng; Ma, Xiong-Feng; Zhu, Zhong-Hong; Zou, Hua-Hong; Liang, Fu-Pei; Langmuir  (2020) –; doi:10.1021/acs.langmuir.9b02990

data_1557282
_publ_section_title
;
 Regulation of the Metal Center and Coordinating Anion of Mononuclear
 Ln(III) Complexes to Promote an Efficient Luminescence Response to
 Various Organic Solvents
;
_journal_name_full               Langmuir
_journal_paper_doi               10.1021/acs.langmuir.9b02990
_journal_year                    2020
_chemical_formula_moiety         'C24 H21 N9 O9 Tb'
_chemical_formula_sum            'C24 H21 N9 O9 Tb'
_chemical_formula_weight         738.42
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2019-05-27
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 111.134(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.6874(6)
_cell_length_b                   10.4401(3)
_cell_length_c                   18.0360(8)
_cell_measurement_reflns_used    3886
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      23.1730
_cell_measurement_theta_min      3.4460
_cell_volume                     2930.9(2)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 15.9784
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
--------------------------------------------------------------------------
  1  \w      6.00  78.00   1.00   15.00    --   17.61-130.00 -76.00   72
  2  \w    -55.00  62.00   1.00   15.00    --   17.61 -19.00-150.00  117
  3  \w     -8.00  90.00   1.00   15.00    --   17.61  38.00-120.00   98
  4  \w    -51.00 -26.00   1.00   15.00    --   17.61 -57.00  90.00   25
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0149917000
_diffrn_orient_matrix_UB_12      0.0044027000
_diffrn_orient_matrix_UB_13      -0.0320696000
_diffrn_orient_matrix_UB_21      0.0424754000
_diffrn_orient_matrix_UB_22      0.0092959000
_diffrn_orient_matrix_UB_23      0.0273198000
_diffrn_orient_matrix_UB_31      0.0068828000
_diffrn_orient_matrix_UB_32      -0.0671411000
_diffrn_orient_matrix_UB_33      0.0016460000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0451
_diffrn_reflns_av_unetI/netI     0.0614
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            15996
_diffrn_reflns_theta_full        25.50
_diffrn_reflns_theta_max         25.50
_diffrn_reflns_theta_min         3.46
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.478
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.73368
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_density_diffrn    1.673
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1460
_refine_diff_density_max         0.948
_refine_diff_density_min         -0.612
_refine_diff_density_rms         0.099
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     417
_refine_ls_number_reflns         5433
_refine_ls_number_restraints     144
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.0781
_refine_ls_R_factor_gt           0.0484
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0589P)^2^+3.1988P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1154
_refine_ls_wR_factor_ref         0.1355
_reflns_number_gt                3691
_reflns_number_total             5433
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            la9b02990_si_002.cif
_cod_data_source_block           20180921_lfp_whf_5aaa
_cod_original_cell_volume        2930.85(19)
_cod_database_code               1557282
_reflns_odcompleteness_completeness 99.67
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Rigid bond restraints
 O4
 with sigma for 1-2 distances of 0.02 and sigma for 1-3 distances of 0.01
3. Uiso/Uaniso restraints and constraints
O1 \\sim O2 \\sim O5 \\sim O8 \\sim O3 \\sim O7 \\sim O4 \\sim O9 \\sim O6:
within 3.8A with sigma of 0.02 and sigma for terminal atoms of 0.01
Uanis(O1) \\sim Ueq, Uanis(O2) \\sim Ueq, Uanis(O5) \\sim Ueq, Uanis(O8) \\sim
Ueq, Uanis(O3) \\sim Ueq, Uanis(O7) \\sim Ueq, Uanis(O4) \\sim Ueq, Uanis(O9)
\\sim Ueq, Uanis(O6) \\sim Ueq: with sigma of 0.02 and sigma for terminal atoms
of 0.01
4. Others
 Fixed Sof: C13(0.5) H13(0.5) C15(0.5) H15(0.5) C12(0.5) H12(0.5) C17(0.5)
 H17(0.5) C16(0.5) H16(0.5) C14(0.5) H14(0.5)
5.a Ternary CH refined with riding coordinates:
 C10(H10), C11(H11), C13(H13), C15(H15), C12(H12), C17(H17), C16(H16), C14(H14)
5.b Aromatic/amide H refined with riding coordinates:
 C23(H23), C20(H20), C26(H26), C9(H9), C24(H24), C6(H6), C3(H3), C25(H25),
 C4(H4), C5(H5)
5.c Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C28(H28A,H28B,H28C)
;
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.530
_oxdiff_exptl_absorpt_empirical_full_min 0.831