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_1557281
_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 H16.5 Eu N9 O9'
_chemical_formula_sum            'C24 H16.5 Eu N9 O9'
_chemical_formula_weight         726.92
_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     dual
_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                 110.828(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.8934(8)
_cell_length_b                   10.4286(4)
_cell_length_c                   17.9567(10)
_cell_measurement_reflns_used    9750
_cell_measurement_temperature    298.94(10)
_cell_measurement_theta_max      27.7460
_cell_measurement_theta_min      2.0430
_cell_volume                     2956.8(3)
_computing_cell_refinement       'CrysAlisPro 1.171.40.14a (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.40.14a (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.40.14a (Rigaku OD, 2018)'
_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    'XT (Sheldrick, 2015)'
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      298.94(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_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     -5.00  33.00   0.50    0.71    --    6.20  37.00 -30.00   76
  2  \w     42.00  79.00   0.50    0.71    --    6.20  37.00 -30.00   74
  3  \w     -8.00  18.00   0.50    0.71    --    6.20 -72.00  82.00   52
  4  \w    -13.00  79.00   0.50    0.71    --    6.20  72.00-147.00  184
  5  \w    -52.00 -26.00   0.50    0.71    --    6.20 -72.00  82.00   52
  6  \w    -11.00  36.00   0.50    0.71    --    6.20 -99.00 120.00   94
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'ROD, Synergy Custom DW system, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0072738000
_diffrn_orient_matrix_UB_12      -0.0463275000
_diffrn_orient_matrix_UB_13      -0.0257291000
_diffrn_orient_matrix_UB_21      0.0395153000
_diffrn_orient_matrix_UB_22      0.0291535000
_diffrn_orient_matrix_UB_23      0.0049398000
_diffrn_orient_matrix_UB_31      0.0201565000
_diffrn_orient_matrix_UB_32      -0.0403572000
_diffrn_orient_matrix_UB_33      0.0331432000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0751
_diffrn_reflns_av_unetI/netI     0.0693
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            21788
_diffrn_reflns_theta_full        25.50
_diffrn_reflns_theta_max         25.50
_diffrn_reflns_theta_min         2.06
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.186
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.00299
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.14a (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_density_diffrn    1.633
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1434
_refine_diff_density_max         1.389
_refine_diff_density_min         -1.250
_refine_diff_density_rms         0.139
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     426
_refine_ls_number_reflns         5444
_refine_ls_number_restraints     720
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.0753
_refine_ls_R_factor_gt           0.0554
_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^)+(0.0990P)^2^+2.2317P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1521
_refine_ls_wR_factor_ref         0.1653
_reflns_number_gt                4072
_reflns_number_total             5444
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            la9b02990_si_002.cif
_cod_data_source_block           l-lfp-whf-1002-300k
_cod_original_cell_volume        2956.8(2)
_cod_original_formula_sum        'C24 H16.50 Eu N9 O9'
_cod_database_code               1557281
_reflns_odcompleteness_completeness 98.67
_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. Uiso/Uaniso restraints and constraints
C00I \\sim C00K \\sim C00L \\sim C00N \\sim C00O \\sim C00P \\sim C00Q \\sim
C00R \\sim C00S \\sim C00T \\sim C00U \\sim C00V \\sim C00W \\sim C00X \\sim
C00Y \\sim C00Z \\sim C010 \\sim C011 \\sim C012 \\sim C013 \\sim C014 \\sim
C015 \\sim C016 \\sim C3 \\sim C4 \\sim C5 \\sim C9 \\sim C6: within 3.8A with
sigma of 0.02 and sigma for terminal atoms of 0.01
Uanis(O002) \\sim Ueq, Uanis(O003) \\sim Ueq, Uanis(O005) \\sim Ueq,
Uanis(O007) \\sim Ueq, Uanis(O00C) \\sim Ueq, Uanis(O00G) \\sim Ueq,
Uanis(O00H) \\sim Ueq, Uanis(O00J) \\sim Ueq, Uanis(O00M) \\sim Ueq: with sigma
of 0.02 and sigma for terminal atoms of 0.01
3. Others
 Fixed Sof: C014(0.5) C015(0.5) C016(0.5) H016(0.5) C3(0.5) C4(0.5) C5(0.5)
 C9(0.5) C6(0.5)
4.a Ternary CH refined with riding coordinates:
 C016(H016)
4.b Aromatic/amide H refined with riding coordinates:
 C00O(H00O), C00P(H00P), C00R(H00R), C00S(H00S), C00U(H00U), C00W(H00W),
 C00X(H00X), C00Y(H00Y), C00Z(H00Z), C013(H013)
4.c Idealised Me refined as rotating group:
 C010(H01A,H01B,H01C), C012(H01D,H01E,H01F)
;
_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 188.160
_oxdiff_exptl_absorpt_empirical_full_min 0.251