Construction and characterization of rare earth complexes for efficient emission tuning by tetraethyl ethylenebisphosphonate and tridentate chelating nitrogen ligands.
Hou, Chuan-Bing; Guo, Gui-Xiong; Dai, Li-Xiong; Li, Ying-Yu; Wang, Lin-Lin; Song, Hui-Hua; Xin, Xiu-Lan; Han, Hong-Liang; Wang, Xue-Dong; Li, Xing-Ru; Jin, Qiong-Hua; Dalton transactions (Cambridge, England : 2003) 54 (2025) 9594–9604; doi:10.1039/d5dt00963d

data_7718767
_publ_section_title
;
 Construction and characterization of rare earth complexes for efficient
 emission tuning by tetraethyl ethylenebisphosphonate and tridentate
 chelating nitrogen ligands.
;
_journal_issue                   24
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              9594
_journal_page_last               9604
_journal_paper_doi               10.1039/d5dt00963d
_journal_volume                  54
_journal_year                    2025
_chemical_formula_moiety         'C40 H46 Ce2 N12 O24 P2'
_chemical_formula_sum            'C40 H46 Ce2 N12 O24 P2'
_chemical_formula_weight         1421.07
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2023-03-13
_audit_creation_method
;
Olex2 1.5
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748)
;
_audit_update_record
;
2024-10-11 deposited with the CCDC.	2025-05-19 downloaded from the CCDC.
;
_cell_angle_alpha                89.8500(10)
_cell_angle_beta                 80.3770(10)
_cell_angle_gamma                88.5100(10)
_cell_formula_units_Z            1
_cell_length_a                   8.00960(10)
_cell_length_b                   9.62580(10)
_cell_length_c                   17.48010(10)
_cell_measurement_reflns_used    12250
_cell_measurement_temperature    293
_cell_measurement_theta_max      74.3110
_cell_measurement_theta_min      5.2560
_cell_volume                     1328.28(2)
_computing_cell_refinement       'CrysAlisPro 1.171.39.33c (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.33c (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.33c (Rigaku OD, 2017)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      293
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.963
_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    -89.00  13.00   0.50    1.00    --    0.00 -19.00  60.00  204
  2  \w    -13.00  89.00   0.50    1.00    --    0.00  19.00 -30.00  204
  3  \w    -13.00  89.00   0.50    1.00    --    0.00  19.00   0.00  204
  4  \w    -89.00  21.00   0.50    1.00    --    0.00 -57.00   0.00  220
  5  \w    -13.00  89.00   0.50    1.00    --    0.00  19.00-180.00  204
  6  \w    140.00 180.00   0.50    1.00    --   94.00  30.00-120.00   80
  7  \w     56.00 106.00   0.50    1.00    --   94.00 -82.00-180.00  100
  8  \w     93.00 132.00   0.50    1.00    --   94.00  30.00-120.00   78
  9  \w     37.00 124.00   0.50    1.00    --   94.00 -82.00  60.00  174
 10  \w     11.00 100.00   0.50    1.00    --   94.00 -82.00 -90.00  178
 11  \w     17.00 111.00   0.50    1.00    --   94.00 -45.00  30.00  188
 12  \w     82.00 160.00   0.50    1.00    --   94.00  15.00-180.00  156
 13  \w     79.00 105.00   0.50    1.00    --   94.00 -82.00 120.00   52
 14  \w      7.00 109.00   0.50    1.00    --   94.00 -15.00 -90.00  204
 15  \w     50.00 116.00   0.50    1.00    --   94.00 -61.00  60.00  132
 16  \w     70.00 113.00   0.50    1.00    --   94.00 -77.00 -60.00   86
 17  \w     92.00 117.00   0.50    1.00    --   94.00 -82.00 -30.00   50
 18  \w     80.00 182.00   0.50    1.00    --   94.00  30.00-150.00  204
 19  \w      7.00 116.00   0.50    1.00    --   94.00 -61.00 -90.00  218
 20  \w      5.00  51.00   0.50    1.00    --   94.00 -77.00 -60.00   92
 21  \w     36.00  83.00   0.50    1.00    --   94.00 -82.00-150.00   94
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC12 (RINC): Kappa dual home/near'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0049241000
_diffrn_orient_matrix_UB_12      0.0322285000
_diffrn_orient_matrix_UB_13      0.0858402000
_diffrn_orient_matrix_UB_21      -0.1218849000
_diffrn_orient_matrix_UB_22      -0.1193772000
_diffrn_orient_matrix_UB_23      0.0253940000
_diffrn_orient_matrix_UB_31      0.1527465000
_diffrn_orient_matrix_UB_32      -0.1016934000
_diffrn_orient_matrix_UB_33      -0.0029025000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0506
_diffrn_reflns_av_unetI/netI     0.0379
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.963
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            15579
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.963
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.486
_diffrn_reflns_theta_min         4.595
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    14.467
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.36424
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.33c (Rigaku Oxford Diffraction, 2017)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.777
_exptl_crystal_description       block
_exptl_crystal_F_000             708
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.346
_refine_diff_density_min         -1.618
_refine_diff_density_rms         0.132
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     363
_refine_ls_number_reflns         5208
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.0362
_refine_ls_R_factor_gt           0.0345
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0709P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0899
_refine_ls_wR_factor_ref         0.0910
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5033
_reflns_number_total             5208
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt00963d2.cif
_cod_data_source_block           lyy-18
_cod_depositor_comments
'Adding full bibliography for 7718766--7718775.cif.'
_cod_database_code               7718767
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C H N O Eu P '
_shelx_estimated_absorpt_t_max   0.276
_shelx_estimated_absorpt_t_min   0.136
_reflns_odcompleteness_completeness 99.50
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C16(H16A,H16B), C19(H19A,H19B), C17(H17A,H17B)
2.b Aromatic/amide H refined with riding coordinates:
 C15(H15), C2(H2), C3(H3), C4(H4), C1(H1), C7(H7), C12(H12), C8(H8), C14(H14),
 C9(H9), C13(H13)
2.c Idealised Me refined as rotating group:
 C18(H18A,H18B,H18C), C20(H20A,H20B,H20C)
;
_shelx_res_checksum              38914
_shelx_hkl_checksum              44620
_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 2.150
_oxdiff_exptl_absorpt_empirical_full_min 0.661