Six-coordinate lanthanide complexes based on bidentate phosphine oxide ligands: synthesis, structure and magnetic properties
Wu, Xiao-Jun; Guo, Hong-Yao; Lin, Wei-Quan; Meng, Yan; Leng, Ji-Dong; Dalton Transactions 54 (2025) 7819–7827; doi:10.1039/D5DT00422E

data_7719001
_publ_section_title
;
 Six-coordinate lanthanide complexes based on bidentate phosphine oxide
 ligands: synthesis, structure and magnetic properties
;
_journal_issue                   19
_journal_name_full               'Dalton Transactions'
_journal_page_first              7819
_journal_page_last               7827
_journal_paper_doi               10.1039/D5DT00422E
_journal_volume                  54
_journal_year                    2025
_chemical_formula_moiety         'C50 H44 Cl2 Er O4 P4, C4 H8 O, Cl'
_chemical_formula_sum            'C54 H52 Cl3 Er O5 P4'
_chemical_formula_weight         1178.44
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2025-04-09
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2025-04-09 deposited with the CCDC.	2025-04-16 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   21.00542(13)
_cell_length_b                   21.75103(16)
_cell_length_c                   22.46591(16)
_cell_measurement_reflns_used    31552
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      70.2210
_cell_measurement_theta_min      3.5140
_cell_volume                     10264.44(12)
_computing_cell_refinement       'CrysAlisPro 1.171.43.144a (Rigaku OD, 2024)'
_computing_data_collection       'CrysAlisPro 1.171.43.144a (Rigaku OD, 2024)'
_computing_data_reduction        'CrysAlisPro 1.171.43.144a (Rigaku OD, 2024)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2017/1 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.991
_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   -124.00   4.00   0.50    0.50    --  -40.39 -14.00 103.00  256
  2  \w     87.00 174.00   0.50    2.50    --   99.00 112.00  56.00  174
  3  \w     39.00  68.00   0.50    2.50    --   99.00  14.00 -85.00   58
  4  \w     47.00  73.00   0.50    2.50    --   99.00-133.00-113.00   52
  5  \w     45.00  91.00   0.50    0.50    --   40.39-125.00 -60.00   92
  6  \w     29.00  71.00   0.50    2.50    --   99.00 -61.00 -60.00   84
  7  \w    110.00 136.00   0.50    2.50    --   99.00 125.00 150.00   52
  8  \w     22.00  53.00   0.50    2.50    --   99.00 -45.00  30.00   62
  9  \w     23.00  52.00   0.50    2.50    --   99.00 -45.00  90.00   58
 10  \w     22.00  49.00   0.50    2.50    --   99.00 -45.00-150.00   54
 11  \w     77.00 104.00   0.50    2.50    --   99.00-125.00  90.00   54
 12  \w    143.00 169.00   0.50    2.50    --   99.00 125.00 150.00   52
 13  \w     28.00  53.00   0.50    2.50    --   99.00 -45.00 -60.00   50
 14  \w     59.00 107.00   0.50    2.50    --   99.00 -77.00  90.00   96
 15  \w     60.00  85.00   0.50    2.50    --   99.00 -94.00 -30.00   50
 16  \w     21.00  47.00   0.50    2.50    --   99.00 -45.00-180.00   52
 17  \w    122.00 176.00   0.50    2.50    --   99.00  45.00 -60.00  108
 18  \w     31.00  61.00   0.50    2.50    --   99.00-125.00  30.00   60
 19  \w     28.00  53.00   0.50    2.50    --   99.00 -45.00 -30.00   50
 20  \w     63.00 117.00   0.50    2.50    --   99.00-135.00  67.00  108
 21  \w     93.00 142.00   0.50    2.50    --   99.00  14.00 -85.00   98
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, DW system, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0135399000
_diffrn_orient_matrix_UB_12      -0.0126249000
_diffrn_orient_matrix_UB_13      -0.0662831000
_diffrn_orient_matrix_UB_21      0.0020725000
_diffrn_orient_matrix_UB_22      0.0697333000
_diffrn_orient_matrix_UB_23      -0.0120258000
_diffrn_orient_matrix_UB_31      0.0719928000
_diffrn_orient_matrix_UB_32      0.0002250000
_diffrn_orient_matrix_UB_33      0.0128929000
_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  0.0469
_diffrn_reflns_av_unetI/netI     0.0366
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            49673
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         70.419
_diffrn_reflns_theta_min         3.525
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    6.028
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.48220
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.43.144a (Rigaku Oxford Diffraction, 2024)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_density_diffrn    1.525
_exptl_crystal_description       block
_exptl_crystal_F_000             4760
_exptl_crystal_preparation       'Magnetic properties'
_exptl_crystal_size_max          0.06
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.03
_refine_diff_density_max         2.977
_refine_diff_density_min         -1.593
_refine_diff_density_rms         0.102
_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     596
_refine_ls_number_reflns         9717
_refine_ls_number_restraints     11
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0450
_refine_ls_R_factor_gt           0.0395
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0496P)^2^+22.7020P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0995
_refine_ls_wR_factor_ref         0.1037
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8581
_reflns_number_total             9717
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt00422e2.cif
_cod_data_source_block           er
_cod_database_code               7719001
_shelx_shelxl_version_number     2017/1
_chemical_oxdiff_formula         ErP5O6Cl3C54H52
_chemical_oxdiff_usercomment     'Er Cl P O C H'
_shelx_estimated_absorpt_t_max   0.840
_shelx_estimated_absorpt_t_min   0.714
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Restrained distances
 O64A-C67A
 2.35 with sigma of 0.01
 C63-O64 \\sim C63A-O64A
 with sigma of 0.02
 C63-C67 \\sim C63A-C67A
 with sigma of 0.02
 O64-C65 \\sim O64A-C65A
 with sigma of 0.02
 C66-C65 \\sim C66A-C65A
 with sigma of 0.02
 C66-C67 \\sim C66A-C67A
 with sigma of 0.02
 C63-C66 \\sim C63A-C66A
 with sigma of 0.04
 C63-C65 \\sim C63A-C65A
 with sigma of 0.04
 O64-C66 \\sim O64A-C66A
 with sigma of 0.04
 O64-C67 \\sim O64A-C67A
 with sigma of 0.04
 C65-C67 \\sim C65A-C67A
 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
Uanis(C63) = Uanis(O64) = Uanis(C66) = Uanis(C65) = Uanis(C67) = Uanis(C67A) =
Uanis(C63A) = Uanis(O64A) = Uanis(C65A) = Uanis(C66A)
4. Others
 Sof(O64A)=Sof(C63A)=Sof(H63C)=Sof(H63D)=Sof(C65A)=Sof(H65C)=Sof(H65D)=
 Sof(C66A)=Sof(H66C)=Sof(H66D)=Sof(C67A)=Sof(H67C)=Sof(H67D)=1-FVAR(1)
 Sof(O64)=Sof(C63)=Sof(H63A)=Sof(H63B)=Sof(C65)=Sof(H65A)=Sof(H65B)=Sof(C66)=
 Sof(H66A)=Sof(H66B)=Sof(C67)=Sof(H67A)=Sof(H67B)=FVAR(1)
5.a Secondary CH2 refined with riding coordinates:
 C4(H4A,H4B), C45(H45A,H45B), C63(H63A,H63B), C65(H65A,H65B), C66(H66A,H66B),
 C67(H67A,H67B), C63A(H63C,H63D), C65A(H65C,H65D), C66A(H66C,H66D), C67A(H67C,
 H67D)
5.b Aromatic/amide H refined with riding coordinates:
 C8(H8), C9(H9), C10(H10), C11(H11), C12(H12), C14(H14), C15(H15), C16(H16),
 C17(H17), C18(H18), C20(H20), C21(H21), C22(H22), C23(H23), C24(H24), C26(H26),
  C27(H27), C28(H28), C29(H29), C30(H30), C34(H34), C35(H35), C36(H36),
 C37(H37), C38(H38), C40(H40), C41(H41), C42(H42), C43(H43), C44(H44), C49(H49),
  C50(H50), C51(H51), C52(H52), C53(H53), C55(H55), C56(H56), C57(H57),
 C58(H58), C59(H59)
;
_shelx_res_checksum              97191
_shelx_hkl_checksum              73814
_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 1.770
_oxdiff_exptl_absorpt_empirical_full_min 0.632