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_1557279
_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 H20 Dy N9 O9'
_chemical_formula_sum            'C24 H20 Dy N9 O9'
_chemical_formula_weight         740.99
_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             2019-06-12
_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                 111.576(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.4862(8)
_cell_length_b                   10.4198(5)
_cell_length_c                   18.1346(9)
_cell_measurement_reflns_used    3643
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      22.7490
_cell_measurement_theta_min      3.7000
_cell_volume                     2896.9(3)
_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 0.998
_diffrn_measured_fraction_theta_max 0.998
_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     35.00  94.00   1.00   20.00    --   17.61 178.00 120.00   59
  2  \w     35.00  94.00   1.00   20.00    --   17.61 178.00  30.00   59
  3  \w    -51.00  38.00   1.00   20.00    --   17.61 -57.00  90.00   89
  4  \w    -50.00  50.00   1.00   20.00    --  -19.80  77.00 150.00  100
  5  \w    -12.00  76.00   1.00   20.00    --   17.61  77.00-150.00   88
;
_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      0.0273901000
_diffrn_orient_matrix_UB_12      -0.0526181000
_diffrn_orient_matrix_UB_13      0.0179102000
_diffrn_orient_matrix_UB_21      0.0078467000
_diffrn_orient_matrix_UB_22      -0.0102241000
_diffrn_orient_matrix_UB_23      -0.0354896000
_diffrn_orient_matrix_UB_31      0.0364448000
_diffrn_orient_matrix_UB_32      0.0419050000
_diffrn_orient_matrix_UB_33      0.0137623000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0693
_diffrn_reflns_av_unetI/netI     0.1131
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            19201
_diffrn_reflns_theta_full        25.50
_diffrn_reflns_theta_max         25.50
_diffrn_reflns_theta_min         3.37
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.645
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.78492
_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    1.699
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1460
_refine_diff_density_max         1.530
_refine_diff_density_min         -0.999
_refine_diff_density_rms         0.137
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.019
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     417
_refine_ls_number_reflns         5377
_refine_ls_number_restraints     302
_refine_ls_restrained_S_all      1.015
_refine_ls_R_factor_all          0.1169
_refine_ls_R_factor_gt           0.0692
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0845P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1660
_refine_ls_wR_factor_ref         0.2035
_reflns_number_gt                2934
_reflns_number_total             5377
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            la9b02990_si_002.cif
_cod_data_source_block           1
_cod_original_cell_volume        2897.0(2)
_cod_database_code               1557279
_reflns_odcompleteness_completeness 99.70
_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
 Dy1, N3
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.001
 Dy1, N4
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.001
3. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 2A with sigma of 0.001 and sigma
for terminal atoms of 0.002
4. Others
 Fixed Sof: C12(0.5) C11(0.5) H11(0.5) C13(0.5) C2AA(0.5) H2AA(0.5) C0AA(0.5)
 H0AA(0.5) C1AA(0.5) H1AA(0.5)
5.a Ternary CH refined with riding coordinates:
 C15(H15), C14(H14), C11(H11), C2AA(H2AA), C0AA(H0AA), C1AA(H1AA)
5.b Aromatic/amide H refined with riding coordinates:
 C6(H6), C16(H16), C9(H9), C5(H5), C4(H4), C3(H3), C21(H21), C22(H22),
 C20(H20), C23(H23)
5.c Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C18(H18A,H18B,H18C)
;
_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 1.323
_oxdiff_exptl_absorpt_empirical_full_min 0.844