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_7718766
_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 La2 N12 O24 P2'
_chemical_formula_sum            'C40 H46 La2 N12 O24 P2'
_chemical_formula_weight         1418.65
_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
_atom_sites_solution_primary     dual
_audit_creation_date             2023-04-17
_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                89.976(2)
_cell_angle_beta                 80.246(2)
_cell_angle_gamma                88.488(2)
_cell_formula_units_Z            1
_cell_length_a                   8.0186(2)
_cell_length_b                   9.6388(2)
_cell_length_c                   17.5457(4)
_cell_measurement_reflns_used    12798
_cell_measurement_temperature    293
_cell_measurement_theta_max      74.0890
_cell_measurement_theta_min      5.1090
_cell_volume                     1336.02(5)
_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 0.995
_diffrn_measured_fraction_theta_max 0.958
_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  21.00   0.50    1.00    --    0.00 -57.00-180.00  220
  2  \w    -13.00  89.00   0.50    1.00    --    0.00  19.00 -90.00  204
  3  \w    -89.00  15.00   0.50    1.00    --    0.00 -37.00  90.00  208
  4  \w    -15.00  89.00   0.50    1.00    --    0.00  37.00  60.00  208
  5  \w    -89.00  15.00   0.50    1.00    --    0.00 -37.00  60.00  208
  6  \w     28.00 111.00   0.50    1.00    --   94.00 -61.00 -60.00  166
  7  \w     89.00 123.00   0.50    1.00    --   94.00 -82.00-150.00   68
  8  \w     12.00  38.00   0.50    1.00    --   94.00 -45.00 150.00   52
  9  \w     92.00 118.00   0.50    1.00    --   94.00 -82.00 120.00   52
 10  \w     72.00 144.00   0.50    1.00    --   94.00  61.00  90.00  144
 11  \w     49.00  80.00   0.50    1.00    --   94.00 -82.00  30.00   62
 12  \w     85.00 113.00   0.50    1.00    --   94.00 -82.00  30.00   56
 13  \w     10.00 115.00   0.50    1.00    --   94.00 -61.00 150.00  210
 14  \w     90.00 124.00   0.50    1.00    --   94.00 -82.00   0.00   68
 15  \w      7.00 123.00   0.50    1.00    --   94.00 -82.00 -60.00  232
 16  \w      5.00 109.00   0.50    1.00    --   94.00 -15.00 -30.00  208
 17  \w     26.00 109.00   0.50    1.00    --   94.00 -15.00-150.00  166
 18  \w     35.00  72.00   0.50    1.00    --   94.00 -82.00  90.00   74
 19  \w     59.00 111.00   0.50    1.00    --   94.00 -45.00 150.00  104
 20  \w     25.00 118.00   0.50    1.00    --   94.00 -82.00 150.00  186
 21  \w      5.00 130.00   0.50    1.00    --   94.00   0.00 -90.00  250
;
_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      -0.1896489000
_diffrn_orient_matrix_UB_12      0.0149521000
_diffrn_orient_matrix_UB_13      -0.0048887000
_diffrn_orient_matrix_UB_21      -0.0170892000
_diffrn_orient_matrix_UB_22      -0.1583082000
_diffrn_orient_matrix_UB_23      0.0085049000
_diffrn_orient_matrix_UB_31      -0.0420801000
_diffrn_orient_matrix_UB_32      0.0166924000
_diffrn_orient_matrix_UB_33      0.0885501000
_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  0.0775
_diffrn_reflns_av_unetI/netI     0.0483
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.958
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            15649
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.958
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.675
_diffrn_reflns_theta_min         4.589
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    13.574
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.59960
_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 colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.763
_exptl_crystal_description       block
_exptl_crystal_F_000             706
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.34
_exptl_crystal_size_min          0.23
_refine_diff_density_max         1.762
_refine_diff_density_min         -1.149
_refine_diff_density_rms         0.110
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     363
_refine_ls_number_reflns         5230
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.0368
_refine_ls_R_factor_gt           0.0351
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0711P)^2^+0.0058P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0954
_refine_ls_wR_factor_ref         0.0961
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5055
_reflns_number_total             5230
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt00963d2.cif
_cod_data_source_block           lyy-17
_cod_depositor_comments
'Adding full bibliography for 7718766--7718775.cif.'
_cod_database_code               7718766
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C H N O P La'
_shelx_estimated_absorpt_t_max   0.146
_shelx_estimated_absorpt_t_min   0.087
_reflns_odcompleteness_completeness 99.58
_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:
 C4(H4), C1(H1), C12(H12), C2(H2), C3(H3), C9(H9), C13(H13), C15(H15),
 C14(H14), C7(H7), C8(H8)
2.c Idealised Me refined as rotating group:
 C20(H20A,H20B,H20C), C18(H18A,H18B,H18C)
;
_shelx_res_checksum              59106
_shelx_hkl_checksum              83999
_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 1.980
_oxdiff_exptl_absorpt_empirical_full_min 0.695